TW205594B - - Google Patents

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TW205594B
TW205594B TW80105777A TW80105777A TW205594B TW 205594 B TW205594 B TW 205594B TW 80105777 A TW80105777 A TW 80105777A TW 80105777 A TW80105777 A TW 80105777A TW 205594 B TW205594 B TW 205594B
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Catalyst co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00—Post-polymerisation treatments
    • C08F6/14—Treatment of polymer emulsions
    • C08F6/22—Coagulation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00—Post-polymerisation treatments
    • C08F6/008—Treatment of solid polymer wetted by water or organic solvents, e.g. coagulum, filter cakes
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00—Developers
    • G03G9/08—Developers with toner particles
    • G03G9/0802—Preparation methods
    • G03G9/0804—Preparation methods whereby the components are brought together in a liquid dispersing medium
    • G03G9/0806—Preparation methods whereby the components are brought together in a liquid dispersing medium whereby chemical synthesis of at least one of the toner components takes place
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00—Developers
    • G03G9/08—Developers with toner particles
    • G03G9/0802—Preparation methods
    • G03G9/0815—Post-treatment

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Developing Agents For Electrophotography (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Polymerisation Methods In General (AREA)

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055^4 Λ 6 13 6 經濟部中央樣準局貝工消费合作社印製 五、發明説明（1 ) 〈發明背景〉 〈發明範圍〉 本發明偽關於一種著色徹粒子之製造方法及一種使用 此方法所産生的著色微粒子之電子攝影甩調色劑。特別乃 關傜一種具有著色劑均勻分散在其中，具有改良的粒子表 面，並可望作為調色劑、塗料、墨水、樹脂楔選物等的箸 色劑之著色微粒子的製造方法以及使用該箸色微粒子製成 的電子攝影用調色劑，當此調色劑兩於諸如雷射印表機或 液晶印表機等印刷裝置時，能産生清晰影像。 本發明偽關於一種自懸浮液中回收主要由樹脂形成的 球狀微粒子之方法。更特定言之，本發明偽關於一種自懸 浮液中有效的回收例如以懸浮聚合法製成的球狀微粒子之 方法。 〈先行技鏟之描述) 電子攝影方法包括在由硒、氯化鋅或硫化鎘等光導性 材料製成的感光材料上形成電子隱藏的影像，以粉末顯影 劑使此隱藏的影像顯影，並將顯出的影像轉印到紙上，固 定紙上的影像。 到目前為止，在電子攝影中用來使隠藏的影像顯影的 調色劑通常是令箸色劑和其它添加物（如電荷控制劑、偏 位預防劑及潤滑劑）溶化、混合並分散到熱塑性樹脂中， 使産生的分散物硬化，磨碎此固體，將産生的粒子加以分 類，並收集所需粒子直徑的著色微粒子。 然而，以上述磨碎步驟來製造調色劑有許多缺點。首 -S- (請先閲讀背面之注意事項再填寫本頁) 本紙張尺度遑用中B國家揉準(CNS)甲4規格(210 X 297公*) A 6 B6 經濟部中央標準局货工消费合作社印製 五、發明説明（2) 先，它需要許多步驟，包括生産樹脂、將此樹脂與箸色劑 及其它添加物混合、磨碎所産生的固體混合物，將産生的 粒子分類並收集所需粒子直徑的箸色微粒子，因此須使用 和這些步驟一樣多的設備。以此種方法所製造的調色劑價 格昂貴是必然的。特別是分類選定本身對於製造粒子直徑 在可使影像形成具高淸晰度而不會有模糊現象的最佳範圍 内的調色劑是不可缺的。因此它有生産效率和g量不足的 問題。其次，在混合的過程中，很難使著色劑和其它添加 物均勻的分散在樹脂中。因此以此種方法製成的調色劑會 有著色劑、電荷控制劑等分散較差的情形，結果是組成粒 子間摩電特性無法均句而不可避免的降低分解程度。在未 來，當關於降低粒子直徑（此為形成高品質影像不可或缺 的）之要求不斷升高而成為這種調色劑的趨勢時，這些問 題會更力Π突顯。現有的研磨設備在使製造此調色劑的粒子 直徑降低的功能上受到限制，即使它們能製造出粒子直徑 降低的調色劑，由此産生的調色劑仍會由於箸色劑和電荷 控制劑的分散較差而有電荷置嚴重不均的問題。 為了消除由上述研磨法製造調色劑所産生的種種缺黑占 ,各種以乳化聚合技術或懸浮聚合技術來製造此種調色劑 的方法已被提出（日本特許公開公報昭36(1961)-10,231 號、昭43(1968)-10,799號、昭 47(1972)-518,305號、昭 51 (1976) -14, 895號等）。這些方法一致是藉箸令擦有箸色 物（如破黑）和其它添加物的聚合單體進行乳化或懸浮聚 合，以一値步驟來合成含箸色物的調色劑。這些方法可使 _4_ (請先閲讀背面之注意事項再填寫本頁} 裝- 線· 本紙張尺專遑用中國《家«準(CNS)甲4規格(210 X 297公*) 05594 Λ 6 13 6 經濟部中央標準局貝工消费合作社印製 五、發明説明（3) 習知的研磨方法之缺點得到相當的改進。由於其中絕不含 研磨步驟，故改進産生的調色劑之易碎程度對它們而言沒 有用處。更進一步言之，由於製成的調色劑的各個粒子為 球形且流動性佳，其具有均勻的摩電特性。然而，以聚合 技術製造調色劑的方法本身也有問題。首先，由於用於聚 合過程中的親水性物質如分散劑和界面活性劑在洗滌步驟 中無法完金去除而持久的殘留在調色劑粒子表面，所産生 的調色劑之電荷性質容易受到環境的影響。其次，由於藉 聚合技術製成的調色劑粒子為球形且表面非常平滑，因此 調色劑會很快的沈積感光材料上且不易除去，結果迫使感 光材料蒙受清除性不佳的困擾。針對這些問題，有許多方 法被提出來，見曰本特許公開公報昭61 (1986) -255,354號 、Β召 53(1978)17,1736 號、BS 63(1988)17,460 號、3召 61(1986)- 1(37,956號等。這些方法並不實用，因為它們 無法産生完全令人滿意的效果，又導致成本增加。 為了解決此類問題，製造具有所需粒子直徑的電子攝 影用調色劑之方法己被掲示，其通常包括：在乳化劑的存 在下將聚合單體、著色劑、和/或磁粉、以及聚合起始物 乳化、分散並聚合，藉此産生一種主要樹脂組合物，在溫 度不超過此主要樹脂組合物的玻璃轉移點中令所産生的聚 合溶液硬化，以不高於此主要樹脂組合物的玻璃轉移點之 溫度加熱硬化産生的粒子，將粒子完全焰解，並將産生的 粒子固體力卩以分類（日本特許公開公報昭61 (1986)-167, 955號、昭 61 (1986) —167, 956號、昭 61 (1986) -5- (請先閲讀背面之注意事項再填窝本頁) 裝· 訂· 本紙張Λ/til用中β Β家«準(CNS)甲4規格(210x297公*) 五、發明説明（4 ) 經濟部中央搮準局與工消费合作社印製 -167, 957號和昭61 (1986) -72, 258號）。 然而，在造些方法中·》由於是以乳化聚合作為主要的 聚合形式，産生的聚合粒子之粒子直徑是靥於次微粒子類 ，且著色劑如确黑並非包含在聚合粒子中，而是固著在聚 合粒子外部。‘即使這些聚合徽粒子經硬化或熱融合的持繽 步驟而形成較大粒子，它們仍無法均句的分散在其中。結 果造成所産生的調色劑有箸色劑分散不均的毛病，而當其 被用作霉子攝影用調色劑時，會引起霣荷不均或消耗調色 劑，可能伴隨著模糊不清的現象或鼓輪表面雜污。以這些 方法進行聚合製成的聚合粒子是如此的小，其粒子直徑須 受控制並在硬化步驟中以不高於此樹脂之玻璃轉移點的溫 度令聚合粒子硬化而增加其粒子直徑。此硬化作用需使用 無機或有機酸當作硬化劑。無論調色劑如何澈底的被洗礎 ，都無法完全除去該硬化劑。殘留的硬化劑會導致調色劑 抗拒黏附在琛境上並迫使調色劑的電性減低。 四、發明之重點： 因此，本發明的目的之一，就是提供一種新頴的箸色 撇粒子製造方法及使用由該方法製成的箸色徹粒子之電子 攝影用調色劑。本發明之更進一步目的，是提供一種具有 箸色劑均勻分散在其中且同時改善粒子表面的著色微粒子 之製造方法。本發明的另一目的傜提供可望用作諏色劑、 塗料、墨水、樹脂模造物等之箸色劑的著色微粒子之製造 方法。本發明的又一目的偽提供一種可用於雷射印表機或 掖晶印表機等印刷設備、産生清晰影像的電子攝影用調色 -6- (請先閲讀背面之注意事項再填寫本頁) 本《•張尺度逍用中國家«準(CNS)甲4規格(210x297公*) Λ 6 136 經濟部中央標準局貝工消#合作社印製 五、發明説明（5) 劑。本發明之更進一步目標，是提供一種自懸浮液中回收 主要由樹脂所形成的球狀微粒子之新穎方法〇本發明的另 一更進一步目的，是提供一種自懸浮液中有效的回收（例 如）以懸浮聚合技術製成的球狀撤粒子之方法。 本發明工作用仁持缠勤勉的研究，企圖克服上述不利 的狀況，已發現藉箸將懸浮聚合産生的球狀著色微粒子經 一集列特殊步驟處理而得到的著色撤粒子完全沒有以上的 問題可有效的用作塗料、墨水及樹脂模造物的箸色劑，更 不必說還有電子攝影用調色劑和使用該著色徹粒子的電子 攝影用調色劑•當其被用於雷射印表機或液晶印表機等印 刷設備時，産生的影像非常清晰，毫無上述問題，本發明 是改良後所得到的結果。 上述之各目標可經由一種生産箸色微粒子的方法來實 現，此方法特點為：在箸色劑和/或磁粉存在下，令聚合 單體懸浮分佈於懸浮介質中，使産生的懸浮液進行懸浮聚 合，利用水為加熱媒介，以5赔11 130=0的溫度範圍對所産 生之平均粒子直徑在涵1150徼米間的球狀箸色微粒子進行 力U熱處理，以使粒子經融合而結塊，再令該塊狀物分解為 平均粒子直徑與融合前大致相同的球狀著色撤粒子。在根 據本發明的箸色徹粒子製造方法中，上述熱處理可在由懸 浮聚合製得的球狀著色微粒子留在水的懸浮介質中時進行 。此外，此種熱處理也可對由懸浮介質中回收的球狀箸色 微粒子塊進行。 在一値較佳的本發明具體實施例中，箸色微粒子的製 -7- (請先閲讀背面之注意事項再填寫本頁) 裝· 訂· 線· 本紙》•尺度逍用中國S家楳準(CNS)甲4規格(210x297公*) Λ 6 Β6 經濟部中央標準局貝工消费合作社印製 -05b9d 五、發明説明（6 ) 造方法包括：在箸色劑和/或磁粉的存在下將聚合單睡懸 浮分布於懸浮介質中，令産生的懸浮液進行懸浮聚合，以 505(198¾的溫度範圍對平均粒子直徑在3到50微米間的球 狀著色撤粒子懸浮物進行加熱處理.藉此催熟聚合反應， 同時經融合而使粒子結塊，再將該塊狀物分解為平均粒子 直徑與融合前大致相同的球狀箸色徹粒子。 在一個更佳的本發明具體赏施例中，著色徹粒子的製 造方法包括：在箸色劑和磁粉的存在下將聚合單體懸浮分 布於懸浮介質中，令産生的懸浮液進行聚合，並在平均粒 子直徑自链肪矿徹米的球狀箸色微粒子之轉化超過90%後 ,(1)在懸浮液中加入不溶於水的撤粒子，（2)以範圍在50 到98”的溫度對産生的混合物進行熱處理，藉以有效的催 熟聚合反應，同時經由融合將球狀著色微粒子轉化為粒子 塊，然後將該塊狀物分解為平均粒子直徑與融合前大致相 同的球狀箸色微粒子。 在另一値本發明的具體實施例中，箸色徼粒子的製造 方法包括：在著色劑和磁粉的存在下將聚合簞體懸浮分布 於懸浮介質中，令産生的懸浮液進行聚合，將所産生之平 均粒子直徑3^150微米間的球狀箸色微粒子自懸浮液中分 離出來，將由此得到的塊狀物在相對溫度7睡(1100^、溫 度50到130T：的狀況下進行熱處理，藉箸融合將粒子轉化 為粒子塊，並將該粒子塊分解為平均粒子直徑與融合前大 致相同的球狀箸色微粒子。 在一個較佳的本發明具體實施例中，著色微粒子的製 -8- (請先閲讀背面之注意事項再場窝本頁) 装· 訂- 線&lt; 本紙張尺度遑用中a 家標準(CNS)甲4規格(210x297公龙) Λ 6 Β6 經濟部中央標準局员工消费合作社印製 五、發明説明（7) 造方法是在箸色劑和/或磁粉的存在下，令聚合單髏懸浮 分布於懸浮介質中，使産生的懸浮液進行聚合，將所産生 之平均粒子直徑在链05峨!味間的球狀著色微粒子自懸浮 液中分離出來，將由此而得到的塊狀物以5蹄U 130”的熱 水進行熱處理，藉融合將粒子轉化為粒子塊，再將該粒子 塊分解為平均粒子直徑與融合前大致相同的球狀箸色徹粒 子。 本發明更進一步指向一種其粒子中念有由上述製造方 法製得的箸色微粒子之電子攝影用調色劑。 本發明也針對一種自懸浮介質中回收懸浮徹粒子的方 法，其特點為將聚合單體懸浮於懸浮介質中，令産生的懸 浮液進行懸浮聚合，在産生的球狀徹粒子之懸浮液中加入 不溶於水的粒子，使得球狀徹粒子凝集，以過減法將球狀 微粒子凝塊自懸浮介質中分離出來。 藉著根據本發明的製造法，可以製造出粒子大小均勻 的箸色微粒子，其具有平整的粒子表面，且懸浮聚合後殘 留的界面活性劑和分散劑的量有顯著的降低，在濕度改變 時其物理性質不會有改變。因此本發明之箸运微粒子可有 效的用作能形成清晰影像且流動性和清除性優異的電子攝 影用調色劑，並可用作塗料、墨水和樹脂模造物的箸色劑 或改良劑。尤其是以上述箸色微粒子製成的本發明之電子 攝影用調色劑，能形成品質優良的影像，且在各種狀況及 不同的時間下均不産生模糊的現象，因此可用於多種電子 攝影設備。其次，本發明中自懸浮介質回收球狀微粒子的 -9- (請先閲讀背面之注意事項再填窝本頁) 装· 訂· 線- 本紙張尺度遑用中國《家«準(CNS)肀4規格(210X297公 Λ 6 13 6 經濟部中央標準局貝工消費合作社印製 五、發明説明（8 ) 方法以普通過濾裝置實現並簡化了固一液分離過程，即使 是由懸浮聚合製得的球狀微粒子之直徑較小。因此•這種 方法有肋於促進以前述方法生産具上述性質之著色撤粒子 的生産力。 〈圖示之簡單説明〉 第1圖是從本發明方法之熱處理步驟中製得的粒子塊 之電子顯微照K。 第2圖是以本發明方法製得的箸色微粒子之電子顯微 照K。 〈本發明較佳具體實例之描述〉 以下將對本發明及其具體實施例有詳細敘述。 •在製造箸色微粒子之本發明方法中，先在加有著色劑 及/或磁粉之情況下，使一種聚合物單體懸浮於懸浮介質 中，並將産生之懸浮液聚合化。由懸浮液聚合得來之著色 球微粒，粒子之平均直徑範圍為3至5¾¾¾米之間，且最好 是3. 5至20微米。此平均粒子直徑範圍，從此發明中利用 熱處理及分解的步驟之觀點上看，有著一極重要之意義。 此二步驟將在下面詳盡描述。由聚合技術而非由懸浮聚合 技術，例如孔化聚合技術，所獲得之聚合粒子，一般之平 均粒子直徑約在0·1微米左右。以熱處理此等較少之聚合 粒子産生之箸色微粒，若以水作為熱處理介質，並將産生 出來之固體粒子分解者比較，無論在粒子形狀及粒子直徑 之分佈上，均顯箸地與利用現時發明方法生産出之粒子不 .同。若此等較小的著色微粒，用作調色劑時，便不能産生 -10- (請先Μ讀背面之注意事项再填窝本頁) 裝- 線. 本紙張疋度遑用中國S家«準(CNS)甲4規格(210x297公址) £05594 Λ 6 Β6 經濟部中央標準局貝工消费合作社印製 五、發明説明（9) 充分滿意的影像。 此種懸浮液聚合法•適用於粒子直徑受調節，或繼绩 同時地調節粒子直徑，更佳的是.在粒子直徑受調節後才 使用此法，粒子直徑之調節作法，乃例如將指定之組成物 ，分散於一水狀介質中，並將其産生之懸浮物，要最少一 次通過一個生産線混合器，例如均句混合器（由Tokushu kika kogyo K*K.製造）或Ebara溫和器（由Ebara Mfg. Co. Ltd製造）。 懸浮聚合法之反應溫度，通常是在攝氏401C至130T： 範圍内進行，且較佳者為50至9010,作用時間則在0*5至 30小時，而2至10小時為較佳。 有效地使用作為懸浮聚合法之聚合性單體成份之聚合 物單體，包括有例如苯乙烯型單體之苯乙燃，0-甲基苯 乙嫌、m-甲基苯乙嫌、p-甲基苯乙嫌、ct —甲基苯乙嫌 、〇-氮化苯乙嫌、m-氣化苯乙嫌及P-氛化苯乙嫌；丙 焼酸或甲基丙嫌酸型單體之甲基丙嫌酸物、乙基丙燃酸物 、正丁基丙嫌酸樹、異丁基丙締酸物、十二基丙嫌酸物、 硬脂酸基丙嫌基物、2-乙基六基丙嫌酸物、甲基甲基丙 嫌酸物、乙基甲基丙嫌酸物、丙基甲基丙嫌酸物、正丁基 甲基丙烯酸物、異丁基甲基丙烯酸物、正八基甲基丙嫌酸 物、十二基丙締酸物、2-乙基六基甲基丙嫌酸物及硬醋 基甲基丙嫌酸物、及乙嫌、丙嫌、丁嫌、氛化乙焼基、醋 酸化乙締基及两嫌#。此等聚合物單體可以單獨地，亦可 以與一或多項之同類型物混用。 - -11- (請先閲讀背面之注意事項再填窝本頁) 本紙張尺度遑用中躏困家《準(CNS)甲4規格(210 X 297公*) Λ 6 13 6 經濟部中央標準局貝工消費合作社印製 五、發明説明（10) 以懸浮法聚合上述之聚合物單驩後，將其生成之撤球 形著色粒子，以下述之情況進行熱處理的話，可將分解之 操作效率改善。如粒子之融合在熱處理時過置地進行，則 分解之操作效率會較差。而當融會不足時·粒子平面的處 理，便不能得到足夠之效果。為了防止過量融合，在懸浮 液聚合過程中，可以採用一種交鍵劑。 在這裡可以發揮效用之交鍵劑，包括芳香族二乙基化 合物例如是二乙基苯、二乙基爸及其衍生物、二乙燦性不 飽和之矮基脂、例如乙烯乙二醇二甲基丙烯酸物、二乙嫌 乙二醇二甲基丙嫌酸物、三乙烯乙二醇甲基丙嫌酸物、三 甲基醇丙焼甲基三丙烯酸物、嫌丙基甲基丙焼酸物、特異 丁基氛基乙基甲基三丙嫌酸物、四乙嫌二乙醇二甲基丙嫌 酸物及1,3-丁烷二醇二甲基丙烯酸；所有之二乙基化合 物，例如Ν,Ν—二乙基苯胺、二乙基酸、硫彳匕二乙基、及 二乙基磺酸、及例如帶有最少三個乙基組之化合物。聚丁 二烯、聚異丙烯、未飽和之聚酯及聚烯類之氛磺化物亦可 有效地被使用。 用來生産球狀著色微粒之箸色劑，可以是任何已知的 染料及色素，而毋需考慮到它們是有機還是無機。在這裡 可以有效地使用之著色劑包括例如硝黑、苯胺黑、苯胺藍 、轉油藍、鉻黃、氯化超海徉藍、杜邦油红、氯条黃、氛 化甲基藍、居太菁藍、草酸化石青、燈黑、油黑、偶気油黑 。如有需要，亦可將上述兩項或以上混合使用。 這裡的磁粉，乃由一種帶有磁性的物質製成。這裡能 -12- (請先閲讀背面之注意事項再蜞窝本頁) 裝· 訂 線· 本紙張尺度边用中a Β家搮準(CNS)甲4規格(210X297公釐) Λ 6 Β6 經濟部中央標準局貝工消費合作社印製 五、發明説明（11) 有效使用的磁粉，包括鐵磁性的金屬如鐵、鈷及錁、和金 屬化合物粉末例如磁鐵礦、赤鐵礦及鐵酸鹽。此等磁粉可 以單獨或者上述箸色劑配合使用。 此箸色劑及/或磁粉可以不經處理使用。若將箸色劑 及/或磁粉，以一合適之方法作表靥處理後才使用，則生 成之著色微粒，便可將箸色劑及，或磁粉均勻地散佈於其 r*T*t •&quot;Γ1。 此等著色徹粉很理想，因為它們産生高質素的影像， 例如當它們作為調色劑使用時，當碳黑被用作為箸色劑時 ，在日本特許公開公報昭63 (1988) —270, 767及昭63 ( 1988) - 265, 913中之磺黑嫁接聚合物，證實是理想的， 這些都在此作參考用。 雖然用於結合在箸色微粒的箸色劑及/或磁粉的數量 ，可以大幅度地改變，以適應不同種類之著色劑及/或磁 粉或適應生産出來的箸色微粒之使用目的，但一般而言， 在重量比為1 : 200的範圍内為理想，而更佳者為重童1 :100 ,基於聚合物單體重量的100份。 以著色劑及/或磁粉産生微粉子時，通常較便利地採 用的方法，是包括準備一帶有著色劑及/或磁粉，溶解或 散佈於其中的聚合物單體，並以懸浮法聚合該聚合物單體 。有時候，此生産法會受到製備球形聚合物粒子時，由於 缺少箸色劑及/或磁粉，固而在利甩適當之溶劑時，令到 球狀聚合粒子吸收了這著色劑及/或磁粉。 可以在懸浮聚合過程中，有效地使用的穩定劑，包括 -13- (請先閲讀背面之注意事项再填窝本頁) 本紙張尺Λ逍用中Β Β家«準(CNS)甲4規格(210x297公 Λ 6 Β6 經濟部中央標準局貝工消費合作社印製 五、發明説明（12) 有水溶性大分子如聚乙焼醇、澱粉、甲基纖維素、駿基甲 基纖維素、m氣乙基纖維素、聚丙烯酸銷及聚甲基丙烯酸 銷，其中可弯效地使用之陰離子表面活化劑，包括一些醋 酸鹽，例如是月桂酸鈉、趙麻子油押驗、焼基礎酸酯鹽、 |磺酸-福馬林凝聚物、聚氣化乙烯烷基酚基_硫酸醋鹽 、及聚氣化乙嫌院基硫酸酯鹽聚合物。 非離子性之表面活化劑，可在此有效地被用者，包括 例如聚氣乙烟院基_類、聚氣化己二稀酸醋、聚氣化乙稀 院基親、甘油酷酸酷，聚氣己嫌齡基酿類、聚氣乙燦酷酸 酯、已二嫌酸酯、及氣化乙嫌—氣化丙嫌塊狀聚合體。 陽離子性之表面活化劑，可在此有效地被用者，包括 有院基胺鹽類，例如有月桂基胺及硬酯基胺乙醋酸化物、 及四次之鞍鹽、例如月桂基三甲基銨鹽。 兩離子性之表面活化劑，有此可適用者，以月桂基二 甲基胺氣化物為代表。 穩定劑應與配方同用，而且它的使用數量，應適當地 調節至生産出來之球狀箸色徽粒，粉子直徑可控制在3至 50微米，而最好是3· 5至2峨^米範圍内。若例如使用一水 溶性大分子作穩定劑時，則此穩定劑之份量，最好是佔重 置0.01%至2090之範圍，而較佳者為0.1%至10%間，視 手聚合物單體之數量而定。 作為聚合過程使用之聚合引發物，可通常地用於懸浮 聚合作闱之任何一油溶性之過氣化物類及偶氡類，均可採 用。這裡可以有效地使甩之聚合作用引發物，包括一些過 -14- (請先閲讀背面之注意事項再填窝本頁) 裝- 訂· 線- 本紙»尺度遑用中B 8家標準(CNS)甲4規格(210X297公*) Λ 6 13 6 經濟部中央搮準扃β：工消费合作社印製 五、發明説明（13) 氣化類引發物例如過氣化苯甲酰、過氣化月桂酰、過氣化 八基院碗i、過氣化鄰位氯化苯申醜、過氣化鄰位甲氣化苯 甲醜、過氣化甲基乙基銅、二異丙基過氣二娥酸、氫過氣 化祜茗、過氣化環六院酮、氣過氣化t-丁基、及氫過氣 化二異三醇苯、2,2 ’ -偶氣-重異丁基腊、2,2 ’ -偶氣-(2,4-二甲基戊基腈）、2,2·—偶氣―重-2,3-二甲基 丁基腈、2,2 —偶気―重—（2_甲基丁基腊）、2,2 —偶 気—重—2,3,3 —三甲基丁基腊、2,2·—偶気—重—（2 —甲基丁基腈）、2,2 —偶氮-重-2,3,3 —三甲基丁基腈 )、2,2·—偶氮—重—2 —異丙基丁基腈、1,1，-偶氮— 重—（琛六院—1 —破化腊、2,2’-偶氣—重一（4-甲基 氣-2,4—二甲基戊基腈、2—(碳醜二胺基—偶氮）異丁 基腊、4,4’ —偶氣—重-4 —氛化戊基酸、2 —(硕酿二胺 基一偶氮）異丁基腈、偶氮-重-4-氡戊基酸、 及二甲基-2,2’ -偶氮-重-異丁基酸化合物。適當之聚 合引發劑使用量，為重置百分之0.1至20的範圍内。最好 是重童的百分之0.1至10，視乎聚合物簞體的數量而定。 由上述聚合物單體成份懸浮液聚合法生産之球狀箸色 微粒子，其中的單體成份，可結合其他聚合物、例如一種 聚脂，然後再於其中，結合適當之已知添加劑，如一種連 鎖轉移劑，以達到調整聚合程度之目的。當此發明之著色 粉子，想用來作一電子攝影用調色劑時，它亦可在其中的 臘及電荷控制劑中以收藏形態産生，只要這些附加物早在 生産時，先於聚合物單體結合置放。其所産生之球狀箸色 -15- (請先閲請背面之注意事項再填窝本頁) 装· 訂· 線· 本紙尺度遑用中团8家«準(CNS)甲4規格（2 U) X 297公;4) Λ 6 B6 經濟部中央標準局貝工消費合作社印製 五、發明説明（Η) 粒子，理想之直徑範圍，是在3至50微米間，較佳者為3* 5 至20微米，而其由粒子直徑變化条數所表逹之粒子直徑分 佈，應在百分之零至八十，而在百分之一至五十間則更佳 。這裡所使用詞句'&quot;粒子直徑變化条數，是指標準偏差， 除以平均粒子直徑後，所獲得之商數百分比。 根據目前發明之生産方法，由懸浮液聚合法所得之球 狀箸色徽粒，以及平均粒子直徑在3至50微米範圍内者， 均利用水作為加熱介質，在攝氏50至130°C範圍内，以熱 處理被轉變為融合的粒子結塊。 這種熱處理可以用懸浮聚合法産生的球狀箸色微粒子 ，在水中作為懸浮介質的狀態下進行。否則，熱處理亦可 以在球狀箸色微粒子的結塊中進行，而結塊會從懸浮介質 中被取走，這種處理的多元性之一，是可以在化合狀態下 進行。這塊從懸浮液介質中取出之球狀箸色微粒結塊，進 行熱處理時之實際方法之一，是將結塊置於一適當的丨呆留 成員上，並用i梓浴形式，将超過上面規定溫度的熱水倒在 結塊上。另一値可以想得到的方法，是例如保留結塊在一 個特定高溫及高溫之情況下。這種熱處理，亦可分別在常 题，減壓或者是力Π壓的狀況下進行。 這種熱處理在對球狀著色徽粒表面的修正來説，是個 極為重要及不可缺少的步驟。設差在這裡所使用的熱水、 溫度低於攝氏50°c的話，球狀替色微粒的融合便完全不會 發生，或只會不足夠地發生，其結果是其表面修正之顯著 效果不能發揮出來，相反地·假如這溫度高於攝氏130°c -16- (請先閲讀背面之注意事項再填窝本頁) 裝&lt; 本紙張尺度遑用中B B家楳準(CNS)甲4規格(210x297公¢) Λ 6 13 6 經濟部中央標準局貝工消费合作社印製 五、發明説明（15) 時，球狀箸色撤粒的融合會過分地進行，以致以後的分解 步驟難以進彳而且所生産的著色微粒，會有一較廣泛的 直徑分佈。 尤其是在第一個模式，熱處理以對球形著色劑懸浮液 進行加熱時，理想的加熱溫度為攝氏50至98的範圍内，較 佳者為65至95度，如此溫度起過98t,融合便會太快地進 行而隨時間失去控制，假如它超過100^：，則融合便需在 —値加壓的情況下進行。 在第一模式中繼續要注意的是，球形著色微粒在懸浮 液聚合溶液之轉換，在理想情況下球形微粒在熱力融合中 應不少於百分之九十，如果轉換率為百分之百，則可採目 前之發明。由於産生懸浮聚合物溶液的時間，及熱處理所 需之溫度，會隨箸轉換之增力Π而增加，這會使熱處理不能 在常壓下有效地進行，而需一個以倒好壓熱器才能達到之 壓力方可進行。此法因而會令未改變之單體之生存，在某 些程度上會較理想。因此從商業角度看，轉換率理想來說 ，應在90%至99.9%之間，較佳者為Q5%至Q9, 9，如轉換 率少於90，由於未轉換之單體將球形著色徽粒塑料化，加 上熱處理亦因邊界表面之表失而致此等微粒之融合，隨著 而來的分解，在令産生之微粒形成與球形箸色微粒在融合 前擁有之粒子直徑看齊時會有一定的困難。一圓粒子之凝 結體，可從球形微粒以懸浮應加熱處理方式取得，因而影 響聚合作用老化，及令未受影嚮之單體聚合，最浚會誘發 球形微粒之融合。 - -17- (請先閲讀背面之注意事項再填窝本頁) 装. 訂- -線， 本紙張尺度遑用中B國家《準(CNS)肀4規格(210X297公*) 經濟部中央標準局具工消费合作社印製 … Λ 6二 05 咖 ____ 五、發明説明〇6) 在第二個模式中，熱處理是進行於在高溫度下，由懸 浮液分離出來之球形微粒結塊上。作為熱處理之高溫度氣 體，溫度最理想是在攝氏至1001間，而包圍著熱處 理地點之太氣濕度，最好是在70%至100%，更佳者為80 至100之範圍之内，如相對濕度少於70%,由於結塊之水 份已蒸發，融合作用會進行得不規則，或者並不能達到所 需之速度。上述之高濃度熱處理•會誘發聚合作用老化· 及未受影響單髏之繼續聚合。在此同時，亦影繼球形箸色 微粒之融合，産生圍狀粒子之凝結體.此高濕度熱處理通 常會進行在2至90分鐘之範圍，更佳者為 5至60分鐘。在 熱處理的第三個模式中，乃以ί堯淋形式，將熱水加到從懸 浮溶液釋出之箸色微粒結塊上，此熱處理使甩之熱水之溫 度，理想範圍是攝氏70它至1001C間。上述之熱水熱處理 ,會誘發聚合作用老化及將未受影響之單體繼續聚合化。 在此同時，亦影嚮著色微粒子之融合，而形成團狀微粒結 塊，熱水熱處理進行時間範圍，一般是在2至90分鐘，較 佳者為5至60分鐘，熱水熱處理可以在1分隔固體/詨體 之設備之進行，例如，一個漏斗或一個離心機，已被用作 從懸浮溶液中取出箸色球形微粒者，在這情況下，要處理 的粒子，可同時以熱水洗濯，而不致影盤此處理。 此等球狀著色微粒，在上述進行之熱處理中會相互融 會。此融合之狀態，可由處理之效果而隨意作調整，為使 以從分解步驟形成之著色微粒，會有一均勻之直徑分佈及 擁有一電子攝影調色劑必需之特性，最佳之融合狀態，是 18- (請先閲讀背面之注意事項再填寫本頁) 裝. 線- 本紙張尺度逍用中國Η家«準(CNS)甲4規格(210X297公*) 0559^ Λ6 13 6 經濟部中央標準局與工消费合作社印製 五、發明説明（Ί7) 粒子分界表靥並不完全消失，而最少有部份殘留。另外， 在力Π熱懸浮液來時對球形著色微粒作熱作用之第一模式熱 處理中，是可以在有需要時加入一種沉澱劑。這會在熱處 理前入懸浮液。此沉澱劑之加入，乃用以促進箸色球形徹 粒之粘合或沉澱，並在熱處理時，對此等粒子之相互融合 有利。同樣地，在第二及棄三種模式中，熱處理是在由懸 浮液中取出之_色球狀微粒之結塊上進行的，因而將球狀 微粒從懸浮液中取出，才加上沉澱劑入懸浮溶液内，去誘 發微粒子粘合或沉澱，是較為有利的，這是因為，以此發 明製出之球形著色微粒，有箸一極小之直徑，在 3至50 徽米之範圍内如上述。因此，若未經過修改，直接從懸浮 液中取出此等粒子是極為困難的。而這個取出過程，如真 的進行則需消耗一大量之能童，或用到一特別設備。懸浮 胶中球形箸色微粒之粘合，就算由融合所得粒子整體密度 之觀點看，或者圍塊從過濾而得之難易程度看，證實是合 乎理想的。 甩作此闱途之沉澱劑，可由已知之沉澱劏中選出，包 括有無機酸及有機酸類，例如草酸，及水溶性金屬鹽類， 例如，由此等酸類及鹼土金屬類形成者，如鋁鹽。使用此 等已知之沉澱劑，需要特別留心，因為它會有機會影繼産 生之球形箸色微粒，在作為電子攝影調色劑時之表現。目 前之發明人，發現此球形箸色微粒之一較差溶劑，在一大 份子之分離或分層時，可作為一沉澱劑，另外亦發現，以 此溶劑産生之球形箸色微粒，可以不帶有以成繫劑形成産 -19- (請先閲讀背面之注意事項再填窝本頁) 本紙張尺度遑用中國8家標準(CNS)甲4規格(210x297公*) 05594 Λ 6 13 6 經濟部中央標準局员工消費合作社印製 五、發明説明（18) 物之缺點。此等輕差之溶劑，包括确氫化物例如己院、庚 烷、辛烷及石油醚、低階醇例如甲醇與乙醇。'&quot;球形箸色 微粒較差溶劑〃之詞句，在這裡使用之意思，是指一種不 能將形成球形著色微粒之樹脂溶解或分佈之溶劑。當然， 上述之較差溶劑或沉澱劑，亦可以跟成絮劑配合使用，除 非發現有不便之情況出現則作別論。 本發明人也發現，當在球狀箸色微粒子的懸浮液中加 入水不溶性微粒子時，就會産生如同使用了已知的絮凝劑 般的穩定絮凝作用，形成所需尺寸的粒子圍，融合工作可 以穩定的進行，而産生的著色徽粒子不會具有使铝絮凝劑 時所製得的産物之缺點。本發明中所使用的水不溶性微粒 子可使球狀著色微粒子的内聚力或融合性維持在最佳狀態 ，顯著的促進粒子園在下一步驟中的可分解性，同時，使 得自分解作用産生的箸色微粒子能顯出高度物理性質。因 止匕，水不溶性微粒子的粒子直徑必須小於球狀箸色徼粒子 。明確的說，它得小於球狀箸色徼粒子直徑的一半。 因此，在一個本發明之較佳具體實施例中，添加此種 水不溶性微粒子到球狀箸色微粒子懸浮液中的手續，是在 球狀著色徹粒子的熱融合步驟或自懸浮液中回收此球狀著 色徽粒子的步驟之前。 在一項本發明之最佳具體實施例中，所採用的步驟包 括：在替色劑和/或磁粉的存在下使聚合單體懸浮分布於 懸浮介質中.令:産生的懸浮液進行聚合，待Q0%以上由此 産生的平均粒子直徑在S到50撤米之球狀箸色徽粒子己轉 -20- (請先Μ讀背面之注意事項再璜寫本頁) 本紙51尺度逍用中a醺家標毕(CNS)甲4規格(210X297公址) Λ 6 13 6 經濟部中央標準局员工消t合作社印製 五、發明説明（19) 化時，（1)在懸浮液中加入水不溶性微粒子，然後（2)以範 圍在50 r：到98 π的溫度對産生的混合物進行熱處理，藉此 催熟聚合作用，同時促進球狀箸色徽粒子的融合而將其轉 化為粒子團，隨後將此粒子團分解為平均粒子直徑與融合 前的球狀著色徽粒子大致相同的粒子。 以下對兩於本發明中作為一種絮凝劑旳水不溶性微粒 子將有明確的敘述。有多種有機粉末與無機粉末可闱作水 不溶性微粒子。 可有效用於本發明中的有機粉末包括交聯及非交聯聚 合物粉末、有機顔料、電简控制齊 11和蠘等物。交聯和非交 聯樹脂粉末包括苯乙嫌型樹脂粉末、丙插酸型樹脂粉末、 甲基丙烯酸型樹脂粉末、聚乙烯型樹脂粉末、聚丙烯型樹 脂粉末、聚5夕氣型樹脂粉末、聚醋型樹脂粉末、聚胺甲酸 乙酯型樹脂粉末、聚醯胺型樹脂粉末、環氣型樹脂粉末、 聚乙烯丁醛型樹脂粉末、松香型樹脂粉末、 烯型樹脂粉 末、酚型樹脂粉末、三聚氯胺型樹脂粉末及鳥糞胺型樹脂 粉末等。可有效用於本發明中的有機顔料包括黃色顔料如 中央黃、 酸黄 S、漢薩（Hansa)黃10G、聯苯胺黃 G、聯苯胺黃GR、腔丨林黃色澱、永久黃NCG和酒石萤 色澱、澄色顔料如鉬撥、永久橙 RK、聯苯胺撥G和陰月· 士林鮮橙GK、红色顔料如永久紅4R 樹脂紅（resor red) 、赃哩口鋼、紅4R、沃丘格（watchnng)紅鈴鹽、色源 紅、鮮洋紅6B、曙紅色i殿、若丹明色ί殿B ^ aza 1 ine lake 和鮮洋红B、紫色顔料如堅牢紫B和甲基紫色澱、藍色染 -21- (請先la讀背面之注意事項再填窝本頁)055 ^ 4 Λ 6 13 6 Printed by Beigong Consumer Cooperative of the Central Bureau of Samples of the Ministry of Economic Affairs 5. Description of the invention (1) <Background of the invention> <Scope of invention> The present invention is about a method for manufacturing colored particles and a method for using the method The electrophotographic toner of the generated colored particles is toner. In particular, Guan Yu is a method for producing colored microparticles having colorants uniformly dispersed therein, having an improved particle surface, and can be expected as a colorant for toners, paints, inks, resin wedges, and the like, and uses the same Toners for electrophotography made of colored particles, when the toner is used in printing devices such as laser printers or liquid crystal printers, can produce clear images. The present invention is about a method for recovering spherical fine particles mainly formed of resin from a suspension. More specifically, the present invention relates to a method for effectively recovering spherical fine particles made by suspension polymerization, for example, from a suspension. <Description of Prior Art Shovel) The electronic photography method includes forming an electronic hidden image on a photosensitive material made of photoconductive materials such as selenium, zinc chloride, or cadmium sulfide, and developing the hidden image with a powder developer, and developing The displayed image is transferred to the paper to fix the image on the paper. So far, the toners used in electrophotography to develop the image of scorpions are usually solubilized, mixed, and dispersed in the toner and other additives (such as charge control agents, deviation prevention agents, and lubricants). In the thermoplastic resin, the generated dispersion is hardened, the solid is ground, the generated particles are classified, and colored fine particles of a desired particle diameter are collected. However, there are many disadvantages in manufacturing the toner with the above grinding step. First-S- (Please read the precautions on the back before filling out this page) This paper is not in the B country (CNS) A 4 specifications (210 X 297 g *) A 6 B6 Cargo worker of the Central Bureau of Standards of the Ministry of Economic Affairs Printed by the Consumer Cooperative V. Description of the invention (2) First, it requires many steps, including the production of resin, mixing this resin with cinders and other additives, grinding the resulting solid mixture, classifying and collecting the particles produced The dust particles are of the required particle diameter, so as many devices as these steps must be used. It is inevitable that the toner manufactured in this way is expensive. In particular, the classification selection itself is indispensable for producing toners with a particle diameter within an optimal range that can form an image with high definition without blurring. Therefore, it has problems of insufficient production efficiency and g quantity. Secondly, during the mixing process, it is difficult to uniformly disperse the colorant and other additives in the resin. Therefore, the toner prepared by this method may have poor dispersion of colorants, charge control agents, etc. As a result, the frictional properties among the constituent particles cannot be uniformly unavoidable and the degree of decomposition is inevitably reduced. In the future, these problems will become more prominent when the demand for reducing the particle diameter, which is indispensable for the formation of high-quality images, becomes a trend for such toners. Existing grinding equipment is limited in the function of reducing the particle diameter of the toner, even if they can produce a toner with a reduced particle diameter, the resulting toner will still be controlled by the toner and charge The dispersion of the agent is poor and there is a problem of serious uneven charge setting. In order to eliminate the various shortages caused by the above-mentioned grinding method for producing toner, various methods for producing such toner by emulsion polymerization technology or suspension polymerization technology have been proposed (Japanese Patent Laid-Open Publication No. Sho 36 (1961)- 10,231, Zhao 43 (1968) -10,799, Zhao 47 (1972) -518,305, Zhao 51 (1976) -14,895, etc.). These methods are consistent with emulsification or suspension polymerization of polymerized monomers that scavenge scintillating materials (such as broken black) and other additives by scintillation, in one step to synthesize scintillator-containing toners. These methods can make _4_ (please read the precautions on the back before filling in this page) 装-线 · This paper ruler only uses the Chinese "Home" standard (CNS) A 4 specifications (210 X 297 public *) 05594 Λ 6 13 6 Printed by the Beigong Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of the invention (3) The shortcomings of the conventional grinding method have been considerably improved. Since the grinding step is never included, the toner produced by the improvement is fragile The degree is not useful for them. Furthermore, since the particles of the manufactured toner are spherical and have good fluidity, they have uniform triboelectric properties. However, the method of manufacturing toner by polymerization technology itself There are also problems. First, because the hydrophilic substances used in the polymerization process, such as dispersants and surfactants, cannot be completely removed in the washing step and remain on the surface of the toner particles for a long time, the charge properties of the generated toner It is easily affected by the environment. Secondly, because the toner particles made by polymerization technology are spherical and the surface is very smooth, the toner will quickly deposit on the photosensitive material and is not easy to remove, resulting in a forced Photosensitive materials are plagued by poor removal properties. In response to these problems, many methods have been proposed, see Japanese Patent Laid-Open Publication No. Sho 61 (1986) -255,354, Beta 53 (1978) 17,1736, BS 63 ( 1988) No. 17,460, 3 Zhao 61 (1986)-1 (37,956, etc .. These methods are not practical because they cannot produce completely satisfactory results and lead to increased costs. In order to solve such problems, manufacturing has required The method of particle diameter toner for electrophotography has been shown, which usually includes: emulsifying, dispersing and polymerizing the polymerization monomer, colorant, and / or magnetic powder, and polymerization initiator in the presence of an emulsifier, by This produces a main resin composition, hardens the resulting polymerization solution at a temperature not exceeding the glass transition point of the main resin composition, and heat hardens the particles at a temperature not higher than the glass transition point of the main resin composition , Completely decompose the particles, and classify the solid particles produced (Japanese Patent Laid-Open Publication No. Sho 61 (1986) -167, 955, Sho 61 (1986) — 167, 956, Sho 61 (1986)- 5- (Please read the precautions on the back before filling the nest page) Binding · Order · This paper Λ / til used in β β home «standard (CNS) A 4 specifications (210x297 g *) V. Invention description (4) Ministry of Economic Affairs Printed by the Central Bureau of Industry and Commerce and Consumer Cooperatives No. 167, 957 and Zhao 61 (1986) -72, 258) However, in the production of these methods,》 was produced due to the main polymerization form of emulsion polymerization The particle diameter of the polymerized particles is lower than that of submicron particles, and the coloring agent is not contained in the polymerized particles, but is fixed outside the polymerized particles. ‘Even if these aggregate emblem particles undergo larger steps of hardening or thermal fusion to form larger particles, they cannot be uniformly dispersed in them. As a result, the resulting toner has a problem of uneven dispersion of the toner, and when it is used as a toner for mold photography, it may cause uneven charge or consumption of the toner, which may be accompanied by blurring. The phenomenon of cleaning or the surface of the drum is dirty. The polymer particles produced by these methods of polymerization are so small that the particle diameter must be controlled and the particle diameter should be increased by hardening the polymer particles at a temperature not higher than the glass transition point of the resin in the curing step. This hardening requires the use of inorganic or organic acids as hardeners. No matter how thoroughly the toner is washed, the hardener cannot be completely removed. The remaining hardener will cause the toner to resist sticking to the environment and force the toner's electrical properties to decrease. Fourth, the focus of the invention: Therefore, one of the objects of the present invention is to provide a new method for manufacturing cerebrum skimming particles and toners for electrophotography using cerebral particles produced by the method. A further object of the present invention is to provide a method for producing colored microparticles having a colorant uniformly dispersed therein while improving the particle surface. Another object of the present invention is to provide a method for producing colored microparticles that can be expected to be used as a colorant for colorants, paints, inks, resin moldings, and the like. Another object of the present invention is to provide a coloring system for electronic photography that can be used in printing equipment such as laser printers or tuck crystal printers to produce clear images-6- (please read the precautions on the back before filling this page ) This "Zhang Scale Xiao uses the Chinese National Standards (CNS) A4 specifications (210x297 g *)) Λ 6 136 Printed by the Central Standards Bureau of the Ministry of Economic Affairs Beigongxiao #Cooperative V. Invention Instructions (5). A further object of the present invention is to provide a novel method for recovering spherical fine particles mainly formed of resin from a suspension. Another further object of the present invention is to provide an effective recovery from a suspension (for example) A method of removing particles in a spherical shape made by suspension polymerization technology. The work of the present invention uses diligent research on humanity to try to overcome the above-mentioned unfavorable conditions. It has been found that the color-removed particles obtained by the spherical colored particles produced by suspension polymerization through a series of special steps are completely free of the above problems. Effectively used as a colorant for paints, inks and resin moldings, not to mention toners for electrophotography and toners for electrophotography using the colored particles • When used in laser printers When printing equipment such as printers or LCD printers, the images produced are very clear, without the above-mentioned problems, and the present invention is the result obtained after improvement. Each of the above objectives can be achieved by a method of producing clinker fine particles. This method is characterized by: suspending and dispersing the polymerized monomer in a suspension medium in the presence of clinker and / or magnetic powder to suspend the resulting suspension Polymerization, using water as the heating medium, and performing heat treatment on the generated spherical dust particles with an average particle diameter of 1150 mm in the temperature range of 5 to 11 130 = 0, so that the particles are agglomerated and agglomerated Then, the mass was decomposed into spherical colored particles with an average particle diameter approximately the same as before fusion. In the method for producing celebrity particles according to the present invention, the above heat treatment may be performed while the spherical colored microparticles prepared by suspension polymerization are left in a water suspension medium. In addition, such heat treatment can also be carried out on the spherical clinker microparticle blocks recovered from the suspension medium. In a preferred embodiment of the present invention, the preparation of celebrity colored particles -7- (please read the precautions on the back before filling in this page) Binding · Order · Thread · This Paper " Standard (CNS) A4 specification (210x297 g *) Λ 6 Β6 Printed by the Beigong Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs -05b9d V. Description of the invention (6) Manufacturing methods include: in the presence of cinder and / or magnetic powder Distribute the polymerized single-sleep suspension in a suspension medium, so that the resulting suspension is subjected to suspension polymerization, and a spherical colored particle suspension with an average particle diameter of 3 to 50 microns is heated by a temperature range of 505 (198¾). In this ripening polymerization reaction, the particles are agglomerated by fusion at the same time, and then the bulk is decomposed into spherical pellets with an average particle diameter approximately the same as before fusion. In a better embodiment of the invention In the method for manufacturing colored particles, the polymerized monomers are suspended and distributed in a suspension medium in the presence of toners and magnetic powder, and the resulting suspension is polymerized. Spherical crimson After the conversion of particles exceeds 90%, (1) add water-insoluble particles to the suspension, (2) heat-treat the resulting mixture at a temperature in the range of 50 to 98 ”to effectively ripen the polymerization reaction, At the same time, the spherical colored microparticles are converted into particle blocks through fusion, and then the block is decomposed into spherical microparticles with an average particle diameter approximately the same as before fusion. In another specific embodiment of the present invention, The manufacturing method of the particles includes: suspending and dispersing the polymeric scatterers in the suspension medium in the presence of the colorant and the magnetic powder, allowing the resulting suspension to polymerize, and producing a spherical scoop with an average particle diameter of 3 ^ 150 microns The colored microparticles are separated from the suspension, and the block thus obtained is subjected to heat treatment at a relative temperature of 7 (1100 ^, temperature 50 to 130T: The block is decomposed into spherical dust-like microparticles with an average particle diameter approximately the same as before fusion. In a preferred embodiment of the present invention, the preparation of colored microparticles-8- (please read the back The Notes field and then nest this page) installed · Order - line &lt; This paper uses the National Standards (CNS) A4 specifications (210x297 male dragons). Λ 6 Β6 Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. 5. Description of invention (7) The manufacturing method is based on / Or in the presence of magnetic powder, the polymerized single skull is suspended in the suspension medium, the resulting suspension is polymerized, and the average particle diameter of the produced is separated from the suspension of spherical colored particles in the chain 05 E! Come out, heat the block thus obtained with 5 hooves U 130 ”hot water, convert the particles into a particle block by fusion, and then decompose the particle block into a spherical custard with an average particle diameter approximately the same as before fusion Selenium particles. The present invention is further directed to a toner for electrophotography in which particles containing celebrite fine particles produced by the above-mentioned manufacturing method are included. The invention is also directed to a method for recovering suspended particles from a suspension medium, which It is characterized by suspending the polymerized monomers in a suspension medium, allowing the resulting suspension to undergo suspension polymerization, and adding water-insoluble particles to the resulting suspension of spherical particles to make the spherical particles completely Particle agglomeration, which separates the spherical microparticle agglomerates from the suspension medium by the subtraction method. By the manufacturing method according to the present invention, it is possible to produce crimson microparticles with uniform particle size, which have a flat particle surface, and after suspension polymerization The amount of residual surfactant and dispersant is significantly reduced, and its physical properties will not change when the humidity changes. Therefore, the microparticles of the present invention can be effectively used to form a clear image and have excellent fluidity and scavengeability Toner for electrophotography, and can be used as a colorant or modifier for paints, inks, and resin moldings. Especially the toner for electrophotography of the present invention, which is made of the above-mentioned microparticles, can form a quality Excellent image, and no blur phenomenon under various conditions and different times, so it can be used in a variety of electronic photography equipment. Secondly, in the present invention, spherical particles -9- are recovered from the suspension medium (please read the back side first Note and refill this page) Binding, Ordering, and Thread-This paper uses the Chinese "Home" standard (CNS) 4 specifications (210X297 ^ 6 13 6 in the Ministry of Economic Affairs Printed by the Beigong Consumer Cooperative of the Bureau of Standards 5. Description of the invention (8) The method realizes and simplifies the solid-liquid separation process with an ordinary filtering device, even if the diameter of the spherical particles made by suspension polymerization is small. The method has the advantage of promoting the productivity of producing colored particles with the above-mentioned properties by the aforementioned method. <Simple description of the diagram> FIG. 1 is an electron micrograph K of the particle block prepared from the heat treatment step of the method of the present invention Fig. 2 is an electron micrograph K of the crimson-colored fine particles prepared by the method of the present invention. <Description of the preferred specific examples of the present invention> The present invention and its specific embodiments will be described in detail below. In the method of the present invention for microparticles, a coloring agent and / or magnetic powder is added to first suspend a polymer monomer in a suspension medium and polymerize the resulting suspension. 5 至 20 微米。 The colored spherical particles obtained by polymerization of the suspension, the average diameter of the particles is between 3 to 5¾¾¾ meters, and preferably 3.5 to 20 microns. This average particle diameter range has a very important meaning from the viewpoint of the steps of heat treatment and decomposition in this invention. These two steps will be described in detail below. The average particle diameter of the polymer particles obtained by polymerization technology rather than suspension polymerization technology, such as pore polymerization technology, is generally about 0.1 microns. The dust particles produced by heat treatment of these few aggregated particles, if water is used as the heat treatment medium, and the resulting solid particles are decomposed, regardless of the distribution of particle shape and particle diameter, they are obviously used. The particles produced by the present invention are different. If these small colored particles are used as a toner, they will not be generated -10- (please read the precautions on the back before filling the nest page). Packing-line. This paper is not used in China. «Public (CNS) A4 specifications (210x297 public address) £ 05594 Λ 6 Β6 Printed by the Beigong Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 5. Invention description (9) Fully satisfactory images. This kind of suspension polymerization method is suitable for adjusting the particle diameter, or adjusting the particle diameter at the same time. It is better to use this method after the particle diameter is adjusted. The adjustment method of the particle diameter is, for example, specified The composition, dispersed in an aqueous medium, and the suspended matter produced by it, should pass through a production line mixer at least once, such as a homojunction mixer (manufactured by Tokushu kika kogyo K * K.) Or Ebara milder ( Manufactured by Ebara Mfg. Co. Ltd). The reaction temperature of the suspension polymerization method is usually carried out in the range of 401C to 130T: and is preferably 50 to 9010, and the action time is 0 * 5 to 30 hours, preferably 2 to 10 hours. Efficient use of polymer monomers as polymerizable monomer components of the suspension polymerization method, including styrene-type monomers such as styrene-type monomers, 0-methyl styrene, m-methyl styrene, p- Methyl phenyl ethyl sulfide, ct-methyl phenyl ethyl sulfide, 〇-nitride phenyl ethyl sulfide, m-gasified styrene acetyl sulfide and P-atmospheric styrene acetyl sulfide; propionic acid or methyl propyl acetoic acid monomer The methyl propionic acid, ethyl propionic acid, n-butyl propionic acid tree, isobutyl acrylic acid, dodecyl propionic acid, stearic acid propionic acid, 2- Ethyl hexapropyl propionate, methyl methyl propionate, ethyl methyl propionate, propyl methyl propionate, n-butyl methacrylate, isobutyl methacrylate, n-octyl Methyl acrylates, dodecyl acrylates, 2-ethylhexalyl methyl acrylates and hard acetate methyl acrylates, as well as B, C, D, A Ethyl group, ethyl acetate group and two suspected #. These polymer monomers may be used alone or in combination with one or more of the same type. --11- (Please read the precautions on the back before filling the nest page) This paper uses the standard "CNS" A4 specifications (210 X 297 g *) Λ 6 13 6 Central Standard of the Ministry of Economy Printed by Jubei Consumer Cooperative Co., Ltd. 5. Description of the invention (10) After polymerizing the above-mentioned single polymer by suspension method, the spherical colored particles produced by it are processed by the following conditions for heat treatment, the operational efficiency of decomposition can be improved . If the fusion of particles is carried out excessively during the heat treatment, the efficiency of decomposition will be poor. When the fusion is insufficient, the processing of the particle plane cannot obtain sufficient effects. To prevent excessive fusion, a cross-linking agent can be used during the suspension polymerization process. The cross-linking agents that can be effective here include aromatic diethyl compounds such as diethylbenzene, diethyldapa and its derivatives, diethylbenzene unsaturated short base grease, such as ethylene glycol di Methacrylic acid, diethyl ethylene glycol, dimethyl propionic acid, triethylene glycol, methyl propionic acid, trimethyl alcohol propane, methyl triacrylate, propyl methyl propane Acids, specific butylamino ethyl methyl tripropyl acid, tetraethyl diethanol dimethyl propyl acid and 1,3-butanediol dimethacrylic acid; all diethyl compounds , Such as Ν, Ν-diethylaniline, diethylacid, diethyl sulfide, and diethylsulfonic acid, and compounds with at least three ethyl groups. Polybutadiene, polyisopropylene, unsaturated polyesters and polyolefinic sulfonates can also be used effectively. The colorant used to produce spherical colored particles can be any known dyes and pigments, regardless of whether they are organic or inorganic. The coloring agents that can be effectively used here include, for example, nitric black, aniline black, aniline blue, oil blue, chrome yellow, chlorinated ultramarine blue, Dupont oil red, chloro strip yellow, atmospheric methyl blue, Jutai Jing blue, oxalated fossil blue, lamp black, oil black, and even oil black. If necessary, two or more of the above can also be used in combination. The magnetic powder here is made of a substance with magnetism. Here can be -12- (please read the precautions on the back before slurring this page) Binding · Threading · This paper is used in the standard side a Β 家 殮 准 (CNS) A 4 specifications (210X297 mm) Λ 6 Β6 Economy Printed by the Beigong Consumer Cooperative of the Central Bureau of Standards of the Ministry 5. Description of the invention (11) Effectively used magnetic powders, including ferromagnetic metals such as iron, cobalt, and tungsten, and metal compound powders such as magnetite, hematite and ferrite . These magnetic powders can be used alone or in combination with the above-mentioned toner. The toner and / or magnetic powder can be used without treatment. If the cyan toner and / or magnetic powder is used after being treated by a suitable method, the resulting colored particles can disperse the cyan toner and / or magnetic powder evenly on its r * T * t • &quot; Γ1. These coloring powders are ideal because they produce high-quality images, such as when they are used as toners, and when carbon black is used as a toner, in Japanese Patent Laid-Open Publication 63 (1988) -270, The sulfonate black grafted polymers in 767 and Zhao 63 (1988)-265, 913 have proved to be ideal, and these are all incorporated herein by reference. Although the quantity of the coloring agent and / or magnetic powder used for binding to the coloring particles can be greatly changed to adapt to different types of coloring agents and / or magnetic powders or the use purpose of the generated coloring particles, but generally In terms of weight ratio, it is ideal in the range of 1: 200, and the better one is Chongtong 1: 100, based on 100 parts of the weight of the polymer monomer. When producing micropowders with colorants and / or magnetic powders, it is usually more convenient to use a method that includes preparing a polymer monomer with colorants and / or magnetic powders dissolved or dispersed therein, and polymerizing the polymer by suspension物 单体。 Material monomer. Sometimes, this production method will be affected by the lack of colorant and / or magnetic powder when preparing spherical polymer particles, so that when the appropriate solvent is thrown away, the spherical polymer particles absorb the colorant and / or magnetic powder . Stabilizers that can be effectively used in the suspension polymerization process, including -13- (please read the precautions on the back side before filling the nest page) This paper size is used in Β home, quasi (CNS) A4 specifications (210x297 Λ 6 Β6 Printed by Beigong Consumer Cooperative of Central Bureau of Standards of the Ministry of Economy V. Description of invention (12) Water-soluble macromolecules such as polyethylene glycol, starch, methyl cellulose, methyl methyl cellulose, m Gas ethylcellulose, polyacrylic acid pin and polymethacrylic acid pin, which can be used flexibly anionic surfactants, including some acetate, such as sodium laurate, Zhao Mazi oil charge test, baked basic acid ester salt , | Sulfonic acid-formalin condensate, poly-gasified ethylene alkylphenol-sulfate acetate, and poly-gasified ethyl sulfate-based sulfate salt polymer. Non-ionic surface active agent can be effective here The used persons include, for example, poly gas ethyl smoke hospital base class, poly gasification adipic acid vinegar, poly gasification ethylene diamine acid base, glycerol acid cooler, poly gas ethyl alcohol base class, poly gas ethyl alcohol cool Acid ester, adipic acid ester, and gasified acetylene—gasified acetylene lumpy polymer. Surfactants that can be effectively used here, including amine salts, such as laurylamine and stearylamine ethyl acetate, and four times saddle salt, such as lauryl trimethyl ammonium salt The two-ionic surfactant, if applicable, is represented by lauryl dimethylamine vapor. The stabilizer should be used together with the formulation, and the amount of its use should be appropriately adjusted to the ball produced. The shape of the color dust is like 3 to 50 microns, and it is best to be in the range of 3.5 to 2 Angstroms. If, for example, a water-soluble macromolecule is used as a stabilizer, the The amount is preferably in the range of 0.01% to 2090, and preferably 0.1% to 10%, depending on the number of monomers in the polymer. As the polymerization initiator used in the polymerization process, it can be usually Any oil-soluble over-vaporized species and even radon species used in suspension polymerization can be used. Here, the polymerization initiator can be effectively thrown off, including some -14- (please read the notes on the back first Matters refill this page) Binding-Binding · Thread-Original Paper »For Standard Use China B 8 Standards (CNS) A 4 specifications (210X297 g *) Λ 6 13 6 Central Ministry of Economic Affairs β: Printed by the Industrial and Consumer Cooperatives 5. Description of the invention (13) Gasification initiators such as pergasification benzene Formyl, over-vaporized lauroyl, over-vaporized Bajiyuan bowl i, over-vaporized ortho-chlorinated benzene benzene succinate, over-vaporized ortho-methyl benzophenone, over-vaporized methyl ethyl copper, Diisopropyl peroxydioleic acid, hydrogen pervaporation Huming, pervaporation cyclohexanone ketone, pervaporation t-butyl, and pervaporation diisotriolbenzene, 2,2 '- A gas-heavy isobutyl wax, 2,2'-a gas- (2,4-dimethylpentylnitrile), 2,2 · —a gas-heavy-2,3-dimethylbutylnitrile 、 2,2 —Euphemia—Heavy— (2_Methylbutyl Wax), 2,2 —Euphemia—Heavy—2,3,3-Trimethylbutyl Wax, 2,2 · —Euphemia— Heavy— (2-methylbutylnitrile), 2,2-azo-heavy-2,3,3-trimethylbutylnitrile), 2,2 · —azo-heavy-2-isopropyl Butyronitrile, 1,1, -azo-heavy— (Chen Liuyuan-1—Broken wax, 2,2′-azo—heavy (4-methyl gas-2,4-dimethylpentane Acrylonitrile, 2— (Carbondiamine-azo) isobutyl wax 4,4 '—azo-heavy-4 —aerated amyl acid, 2-((diaminodiamino-azo) isobutyl nitrile, azo-heavy-4- radon amyl acid, and dimethyl Yl-2,2'-azo-heavy-isobutyl acid compound. The appropriate amount of polymerization initiator used should be within the range of 0.1 to 20 percent reset. Preferably, it is 0.1 to 10 percent of the heavy child, depending on the number of polymer molds. Spherical clinker colored microparticles produced by the above-mentioned polymer monomer component suspension polymerization method, in which the monomer component can be combined with other polymers, such as a polyester, and then combined with appropriate known additives such as a Chain transfer agent to achieve the purpose of adjusting the degree of polymerization. When the colored powder of this invention is intended to be used as a toner for electrophotography, it can also be produced in the form of a collection in the wax and charge control agent, as long as these additives are produced before the polymerization The monomers are placed together. The resulting spherical dust color -15- (please read the precautions on the back and fill the nest page first). Pack · Order · Thread · Use this paper standard to use 8 squadrons (CNS) A4 specifications (2 U) X 297 g; 4) Λ 6 B6 Printed by Beigong Consumer Cooperative of Central Bureau of Standards of the Ministry of Economy V. Invention description (H) Particles, the ideal diameter range is between 3 and 50 microns, preferably 3 * 5 to 20 microns, and the particle diameter distribution represented by the number of particle diameter changes should be between 0 and 80 percent, and more preferably between 1 and 50 percent. The phrase '&quot; particle diameter change number used here refers to the standard deviation, divided by the average particle diameter, the percentage of the quotient obtained. According to the production method of the present invention, the spherical dust-shaped emblems obtained by the suspension polymerization method, and those with an average particle diameter in the range of 3 to 50 microns, use water as the heating medium in the range of 50 to 130 ° C , Agglomerated by heat treatment into fused particles. This heat treatment can be carried out in the state of spherical clinker-like fine particles produced by suspension polymerization in a state where water is used as a suspension medium. Otherwise, the heat treatment can also be carried out in the agglomerates of spherical dust particles, and the agglomeration will be removed from the suspension medium. One of the versatility of this treatment can be carried out in a combined state. This spherical agglomerate particle agglomerated from the suspension medium is one of the practical methods of heat treatment. It is to put the agglomerate on a suitable member and use the bath to exceed the above. The hot water of the specified temperature is poured on the cake. Another conceivable method is, for example, to keep the agglomeration at a specific high temperature and high temperature. This heat treatment can also be carried out under normal conditions, under reduced pressure or under pressure. This heat treatment is an extremely important and indispensable step in the correction of the surface of the spherical colored emblem. If the hot water used here is set at a temperature lower than 50 ° C, the fusion of spherical color-changing particles will not occur at all, or it will only occur insufficiently. As a result, the significant effect of the surface correction cannot be Play it out, on the contrary · If this temperature is higher than 130 ° C -16- (please read the precautions on the back before filling the nest page) &lt; The size of this paper is in the form of BB Family Standard (CNS) Grade 4 (210x297 g) Λ 6 13 6 When the invention description (15) is printed by the Beigong Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs, the spherical grate The fusion of the color-removing particles will be excessively performed, so that the subsequent decomposition steps are difficult to carry out and the colored particles produced will have a wider diameter distribution. Especially in the first mode, when the heat treatment is used to heat the spherical colorant suspension, the ideal heating temperature is in the range of 50 to 98 degrees Celsius, preferably 65 to 95 degrees Celsius. It will proceed too quickly and lose control over time. If it exceeds 100 ^ :, the fusion needs to be carried out under pressure. In the first mode, we should continue to pay attention to the conversion of spherical colored particles in the suspension polymerization solution. Ideally, the spherical particles should be not less than 90% in thermal fusion. If the conversion rate is 100%, then Take the current invention. Since the time to produce the suspended polymer solution and the temperature required for the heat treatment will increase with the increase in the conversion of the chopsticks Π, this will prevent the heat treatment from being carried out effectively under normal pressure, and it needs an inverted autoclave to achieve it Pressure can only be carried out. This method will therefore allow the survival of the unaltered monomer to some extent to be ideal. Therefore, from a commercial point of view, the conversion rate should ideally be between 90% and 99.9%, preferably Q5% to Q9, 9. If the conversion rate is less than 90, the spherical colored emblem Plasticization of the particles, combined with heat treatment, also results in the fusion of these particles due to the loss of the boundary surface. With the subsequent decomposition, the resulting particles will form the same diameter as the spherical clinker particles before the fusion. There are certain difficulties. The condensate of a round particle can be obtained from the spherical particles in suspension and should be heated, which affects the aging of the polymerization and polymerizes the unaffected monomers, and most will induce the fusion of the spherical particles. --17- (Please read the precautions on the back before filling the nest page) Binding. Binding-This paper uses the standard of China National Standard "CNS" 4 (210X297) * Central Standard of the Ministry of Economy Printed by the Bureau Cooperative Consumer Cooperative Society ... Λ 6 二 05 Coffee ____ V. Description of invention 〇6) In the second mode, heat treatment is carried out on agglomerates of spherical particles separated from the suspension at high temperatures. As a high-temperature gas for heat treatment, the temperature is ideally between 100 degrees Celsius and 1001, and the humidity of the atmosphere surrounding the heat treatment site is preferably 70% to 100%, more preferably 80 to 100, such as The relative humidity is less than 70%. Because the agglomerated water has evaporated, the fusion will proceed irregularly, or the desired speed cannot be achieved. The above-mentioned high-concentration heat treatment will induce polymerization aging and the continued polymerization of unaffected single skulls. At the same time, it also follows the fusion of spherical dust particles to produce agglomerates of surrounding particles. This high-humidity heat treatment is usually carried out in the range of 2 to 90 minutes, more preferably 5 to 60 minutes. In the third mode of heat treatment, hot water is added to the agglomerates of celebrity particles released from the suspended solution in the form of ί Yaolin. This heat treatment makes the temperature of the hot water thrown, the ideal range is 70 degrees Celsius. Between 1001C. The above hot water heat treatment will induce polymerization aging and continue to polymerize unaffected monomers. At the same time, it also affects the fusion of colored particles to form agglomerates of agglomerated particles. The time range of hot water heat treatment is generally 2 to 90 minutes, preferably 5 to 60 minutes, hot water heat treatment can be at 1 The equipment for separating solids / carcasses, for example, a funnel or a centrifuge, has been used to remove the spherical spherical particles from the suspension solution. In this case, the particles to be treated can be washed with hot water at the same time , Without causing this process. These spherical colored particles will fuse with each other during the heat treatment described above. The state of this fusion can be arbitrarily adjusted by the effect of the treatment. In order to make the colored particles formed from the decomposition step have a uniform diameter distribution and possess the characteristics necessary for an electrophotographic toner, the optimal fusion state is 18- (please read the precautions on the back before filling in this page) Pack. Thread-This paper size is easy to use Chinese Η home «quasi (CNS) A 4 specifications (210X297 public *) 0559 ^ Λ6 13 6 Central Bureau of Standards of the Ministry of Economic Affairs Printed with industrial and consumer cooperatives. 5. Description of Invention (Ί7) The particle boundary surface does not completely disappear, and at least part of it remains. In addition, in the first mode of heat treatment that heats the spherical colored particles when the thermal suspension comes, it is possible to add a precipitant if necessary. This will enter the suspension before heat treatment. The addition of this precipitating agent is to promote the adhesion or precipitation of the spherical colored pellets, and it is beneficial to the fusion of these particles during heat treatment. Similarly, in the second and third modes, the heat treatment is carried out on the agglomerates of chromatic spherical particles taken out of the suspension, so the spherical particles are taken out of the suspension before the precipitation agent is added. In the suspension solution, it is more advantageous to induce the adhesion or precipitation of fine particles. This is because the spherical colored particles produced by this invention have a very small diameter, which is in the range of 3 to 50 nm as described above. Therefore, it is extremely difficult to remove these particles directly from the suspension without modification. However, if this removal process is really carried out, a large amount of energy is required, or a special device is used. The adhesion of the spherical dust particles in the suspension gel, even from the point of view of the overall density of the particles obtained by fusion, or the ease of filtration from the surrounding block, proved to be ideal. The precipitating agent used in this process can be selected from known precipitating agents, including inorganic acids and organic acids, such as oxalic acid, and water-soluble metal salts, for example, those formed from such acids and alkaline earth metals, such as aluminum salt. The use of these known precipitating agents requires special attention, as it will have the opportunity to affect the performance of the spherical scintillating particles that are produced as an electrophotographic toner. The present inventors have found that one of the spherical cinder-colored particles is a poor solvent, which can be used as a precipitating agent when a large part of the particles is separated or layered. In addition, it has also been found that the spherical cinder-colored particles produced by this solvent can be used without It is produced with a synergist-19- (Please read the precautions on the back before filling the nest page) This paper uses the Chinese 8 standard (CNS) A 4 specifications (210x297 g *) 05594 Λ 6 13 6 Economy Printed by the Ministry of Central Standards Bureau's Employee Consumer Cooperative V. Invention Description (18) The shortcomings of things. Such poor solvents include hydrides such as hexane, heptane, octane and petroleum ether, and lower alcohols such as methanol and ethanol. '&quot; Spherical cinder-colored particles are poor solvents. The term used here refers to a solvent that cannot dissolve or distribute the resin that forms spherical colored particles. Of course, the above-mentioned poor solvents or precipitants can also be used in conjunction with flocculants, unless the inconvenience is found. The present inventors also found that when water-insoluble fine particles are added to the suspension of spherical dust-like fine particles, a stable flocculation effect like the use of a known flocculant is generated, forming a particle circumference of a desired size, and fusion work It can be carried out steadily, and the colored emblem particles produced will not have the disadvantages of the products made by the aluminum flocculant. The water-insoluble microparticles used in the present invention can maintain the cohesiveness or fusion of the spherical colored microparticles in the best state, significantly promote the decomposability of the particle garden in the next step, and at the same time, make the color generated by the self-decomposition Microparticles can exhibit a high degree of physical properties. Because of the dagger, the particle diameter of the water-insoluble microparticles must be smaller than the spherical cymbal particles. Specifically, it must be less than half the diameter of the spherical pellet. Therefore, in a preferred embodiment of the present invention, the procedure for adding such water-insoluble microparticles to the suspension of spherical microparticles is to recover this from the thermal fusion step of the spherical colored particles or from the suspension Spherical colored emblem particles before the step. In a preferred embodiment of the present invention, the steps used include: suspending and dispersing the polymerized monomer in the suspension medium in the presence of color-shifting agent and / or magnetic powder. Order: the resulting suspension is polymerized, After the Q0% or more of the resulting average particle diameter is between S and 50 meters, the spherical crimson emblem particles have been turned to -20- (please read the precautions on the back before writing this page). a 鈺 家 标 毕 (CNS) A 4 specifications (210X297 public address) Λ 6 13 6 Printed by the employee cooperative of the Central Standards Bureau of the Ministry of Economic Affairs V. Description of the invention (19) When it is changed, (1) add water to the suspension Insoluble fine particles, and then (2) heat-treat the resulting mixture at a temperature ranging from 50 r: to 98 π, thereby aging the polymerization, and at the same time promoting the fusion of the spherical crimson emblem particles and converting them into particle clusters, This cluster is then decomposed into particles with an average particle diameter approximately the same as the spherical colored emblem particles before fusion. The two water-insoluble fine particles used as a flocculant in the present invention will be described clearly below. There are a variety of organic powders and inorganic powders that can be used as water-insoluble fine particles. Organic powders that can be effectively used in the present invention include cross-linked and non-cross-linked polymer powders, organic pigments, electronically controlled Qi 11 and worms. The cross-linked and non-cross-linked resin powders include styrene-type resin powders, acryl-type resin powders, methacrylic resin powders, polyethylene-based resin powders, polypropylene-based resin powders, poly-five-type resin powders, Polyvinyl resin powder, polyurethane resin powder, polyamide resin powder, ring gas resin powder, polyvinyl butyral resin powder, rosin resin powder, vinyl resin powder, phenol resin powder , Melamine resin powder and Guanoamine resin powder, etc. Organic pigments that can be effectively used in the present invention include yellow pigments such as central yellow, acid yellow S, Hansa yellow 10G, benzidine yellow G, benzidine yellow GR, cavity yellow lake, permanent yellow NCG and wine Stone fluorescing lake, clear pigments such as molybdenum dial, permanent orange RK, benzidine dial G and Yinyue · Shilin fresh orange GK, red pigments such as permanent red 4R resin red (resor red), shuanglikou steel, red 4R , Watchchng (watchnng) red bell salt, color source red, bright magenta 6B, dawn red i hall, rhodamine bright color hall B ^ aza 1 ine lake and bright magenta B, purple pigments such as fast violet B and methyl Purple Lake, Blue Dye-21- (please read the notes on the back before filling the nest page)

本紙張尺度逍用中S 8家標準(CfNS)甲4規格（2丨0x297公¢) 經濟部中央搮準扃员工消f合作社印製 Λ 6 ______J36_ 五、發明説明（20) 料如^性藍色灘、維多利亞藍色i殿、誌氣藍、非金屬歌氣 藍、酞氡藍的部分氛化物、堅牢天藍和#滿藍BC、以及 綠色顔料如%色 B、孔雀線色殿和法納爾（Fanal )黃 縐G等。可有效用於本發明中的電荷控制劑包括苯胺里、 單偶氮染料、鈴、號泊酸十六酯、%甲酸的烷基酯和院基 醯胺類、硝腐植酸、 Ν,Ν -四申基二胺二苯甲銅、Ν,Ν -四甲基聯苯胺、三tyq、和柳酸的金屬錯合物等在電子 攝影領域中被稱為帶電控制劑的樹質之粉末。可有效周於 本發明中的蠘類物質包括具有從 80 r：到：LSO r的琛形 軟化點的聚合物粉末、溶點在70 °C到60 C的高悠點石鱲 、脂酸酯及其部分皂化的衍生物、高脂肪酸、脂肪酸的金 屬鹽類、和高級醇。 可有效用於本發明中的無機粉末包括鋁、二氣化鈦、 鈦酸銷、鈦酸鋒、鈦酸鈣、欽酸總、氣化鮮、矽砂、白土 、雲母、平片晶石、矽土、各種無機氣化樹顔料、二氯 化鉻、二氧化鋪、鐵紅、二氣化銻、氣化鎭、氣化錯、硫 酸鋇、硕酸銷、破酸經、砂石、硝化矽、氮化砂、磺化硼 、硕化鎢、硕化鈦和硕黑等的微子或顋粒。 在以上所提到的水不溶性粉末中，其疏水指數（Μν/ : 甲醇可濃性）在5以上者特別合思，因為它們能賦予由分 解作用製得的球狀徽粒子理想的防潮性。當球狀微粒子被 用作電子攝影雨調色劑時，它們也顯示出有助於電荷穩定 性。上述特別適用的水不溶性粉末包括多種無機氯化物如 砂、鈦和銳、其己進行處理以分辨碩黑如開正（Ketjen) -22- &lt;請先閲讀背面之注意事項再填寫本頁) 装&lt; 订 本紙Λ尺度边用中a a家《率(CNS)TM規格(210X297公;¢) Λ 6 Β6 經濟部中央標準局貝工消費合作社印製 五、發明説明（2Π) 黑、乙炔墨和爐黑的疏水性和導電性種類。 本文中所使用的「疏水指數」一詞是參考由以下步驟 中得到的數值。 (1) 在一内容量為200毫升的燒杯中放入0· 2克 給定的樣品，以50毫升純水稀釋。 (2) 以磁性攪拌器持續攪拌樣品水溶液，並將甲 醇加入携拌溶液的表面之下〇 (S)將攪泮溶掖表面看不到樣品的時刻作為測試 終黑占。 (4)根據以下方程式，以測試中耗去的甲醇量計 算^出樣品水度。 疏水指數（％)=【X/ (50+X) } X100 其中X代表甲醇的甩量（毫升）。 考慮到産生高解像力所需小粒子直徑調色劑的電荷穩 定性，本發明中選闱的水不溶性微粒子需具有導電性。可 有效應、甩於本發明中的可導電水不溶性微粒子包括可導電 的破黑、二氣化鈦和氣化錫加上氣化錄、可導電的氣化金辛 和欽黑等的粉末。 為了有效的逵成上述目標，此種水不溶性微粒子的粒 子直徑須在0.001到10微米之間，以在0· 005到5微粒之間 較佳。假使水不溶性徽粒子的粒子直徑未超過0. 001徽米 .可能會使得加入這些粒子能産生的效果，即顯著增進絮 凝性質、分解性、流動性、清除性等當箸色微粒子被用作 電子攝影用調色劑時所能顯示出的特性不再出現。相反的 - 2怂- (請先閲讀背面之注意事項再填窝本頁) 裝· -線- 本紙張Λ羊遑用中a國家楳毕(CNS)甲4規格(210&gt;&lt;297公货) 五、發明説明（22) 經濟部中央標準局貝工消費合作社印製 ，如果水不溶性微粒子的粒子直徑超過10微米，則可能使 添加這些粒子所産生的效果非常低，且當箸色撤粒子被用 作電子攝影用調色劑時所應産生的解像力之改進也不會出 現。這些水不溶性微粒子的添力Π量選擇範圍相當廣，視所 用之水不溶性徽粒子之種類及粒子直徑而定。若用童非常 小，添加這些粒子很難顯出效果。若用量非常大，則當箸 色徽粒子用作電子攝影用調色劑時，可能會有電荷性質及 \ 環境穩定性方面的副作用。因此，添力卩量在0· 01到10糾分 重量比範圍内較佳，0· 1至U50份重量比最佳-以聚合單體 組合物為100份重量比。上面所提到的各種水不溶性徹粒 子可單獨或以二或多種形成混合物供使甩。不消說，甚至 當使用了水不溶性微粒子時，也可以同時使用上述已知的 絮凝劑或痣溶劑來製造球狀著色微粒子，除非合併使用會 帶來不便，通常，可能添加一種適當的有機溶劑以促進融 合作用。 由於添力Π上述種類的水不溶性微粒子到水性懸浮液中 而引起的球狀著色微粒子之内聚或沈降作用，是將此添加 物加入球狀箸色微粒子的懸浮掖中並令産生的混合物在擬 拌而不需額外加熱的狀態下放置指定的一段時間而産生的 。在本發明生産著色微粒子的方法中，供應在指定範圍之 内的熱源沒有任何問題，因為自懸浮聚合中産生的球狀著 色徽粒子已成為相互融合狀態，特別是粒子彼此融合而末 完全失去其界面的狀態。明確的説，當以上述第一種方式 加熱球狀箸色徽粒子的懸浮液來進行球狀箸色徼粒子融合 -24-- (請先閲讀背面之注意事項再填窝本頁) 本紙張尺度逍用中B B家«毕(CNS&gt;T4規格(210x297公*) Λ 6 Β6 經濟部中央標準局兵工消t合作社印製 五、發明説明（23) 的熱處理時，可在加入水不溶性微粒子後以501C到130T： 範圍内的溫度進行加熱，球狀箸色撤粒子的内聚以至於融 合作甩，便可持續展開。鲎如上述第二或第三種方式，對 取自懸浮介質的球狀箸色撤粒子塊進行融合球狀箸色微粒 子的熱處理時，可在内聚處理的短時間内以在50^：到130 r：範圍内或以下的溫度進行力π熱，使取自懸浮液的塊狀凝 集體中的融合狀態達到某種程度。 在上述第一種方式中，融合球狀箸色徼粒子的熱處理 方式是對其懸浮液力Π熱，此例中自懸浮液内取得由球狀著 色徽粒子融合而産生的粒子圍之方式是使用普通的固體一 液體分離裝置-利用吸引過濾、加壓過濾或離心過濾的原 理。在粒子圍中所産生的融合狀態最好能使融合産物具有 0· 1到0· 9克/立方公分的體密度，以0·廷丨伯* 7克/立方公 分最佳。雖然粒子圃的形狀或大小並無限制，但其最好能 形成平均尺寸在20到10, 000微粒的粒子，以30到1, 00印敢 米最佳，這是考慮到便於在熱融合處理後進行過總、乾燥 及分解等工作。若其尺寸小於20微米，則粒子的回收需消 耗非常大的能量或使闱特殊裝置。若其尺寸超過10, 000徽 米，則分解時需要巨大的能量。其後由上述得到之粒子圃 便經由乾燥的步驟而進行到分解步驟。 在上述第二和第三種方式中，為了融合球狀箸色微粒 子，是對取自懸浮介質的球狀著色徼粒子塊進行熱處理， 最好是使球狀箸色微粒子互相内聚變成微粒子凝集體，以 為隨後將球狀著色微粒子自懸浮介質中分離出來作準備， -25- (請先閲讀背面之注意事項再填寫本頁) 裝- 訂- 線- 本紙張尺本遴用中國Η家標準(CNS)甲4規格(210x297公龙) Λ 6 13 6 經濟部中央標準局貝工消費合作社印製 五、發明説明（24) 如此有助於以普通的固液分離設備來進行分離。此微粒子 凝集體之髏密度最好是在0· 05到0·9克/立方公分範圍内 ，以0.1到0· 7克/立方公分最佳。雖然微粒子凝集體 的形狀和尺寸並無限制，但其最好能生成平均尺寸在2涵11 10, 000微米的粒子，以30到1,00ΘΜ米較佳，這是考慮到 便於在熱融合處理後進行過減、乾燥及分解等工作。在這 些方式中，上述的熱處理是對如上所述回收的球狀著色微 粒子塊進行，結果得到由球狀箸色微粒子融合而形成的粒 子園。融合的狀態最好能使粒子圍具有1到0· 9克/立方 公分的體密度，以0·2®Ι0·7克/立方公分最佳。如同在上 述第一方式中的方式，粒子園經由乾燥的步驟而進行到分 解步驟。 在分解步驟中，乾燥狀態的粒子園被分解為平均粒子 直徑與融合前大致相同的球狀箸色微粒子。可使用任何曾 用作粒子和頼粒之工業生産的研磨設備來進行分解作用。 在理想方式中，分解為平均粒子直徑與融合前的球狀 箸色微粒子大致相等的作用（如列於本文中供參考者）具 備了使得自融合球狀箸色微粒子的粒子園中之個別粒子成 為未完金失去其界面的程度（如第1圖放大明倍之電子掃 描顯微照相中清晰顯示的），分解為融合前簞一的球狀箸 色撤粒子，結果使各個粒子圍中的粒子回復到在分解前球 狀著色微粒子僅僅變形的狀態。然而，的確很難控制使界 面融合狀態均勻。如第2ΙΜ電子掃描顯微照相（1500倍） 中所清晰顯示的，所欲製造的著色撤粒子通常是以徽粒子 .-26- (請先閲讀背面之注意事項再墦寫本頁) 裝- 訂· 線&lt; 本紙張尺度逍用中困Η家標準(CNS)甲4規格(210X297公釐) 1.0559^ Λ 6 Β6 經濟部中央標準局员工消费合作社印製 五、發明説明（25) 混合物的型態産生的，此混合物是在融合和分解前球狀著 色撤粒子變形且破裂，而碎Κ黏附在變形的粒子上所産生 的。甚至當一批著色微粒子是上述之混合物時，其品質也 決不比理想型箸色微粒子差，只要此球狀著色微粒子混合 物的平均粒子直徑和融合及分解前的球狀著色微粒子大致 相等。在此例中，當箸色微粒子之平均粒子直徑的變化率 在球狀箸色撤粒子的20%之內（以10¾之内較佳，5 %之 内更理想），則著色微粒子及球狀箸色微粒子的平均粒子 直徑可視為大致相同。 由上述方式生産的著色撤粒子之粒子直徑與其粒子直 徑之分佈情形已如所需的受到控制。然而理想的粒子直徑 範圍是在涵115峨5[米間，以3.涵U20撒米最佳，且平均粒 子直徑的分佈為其粒子直徑變異傜數在0到80^的範圍内 ，以睡1150%較佳。此處「粒子直徑變異偽數」一詞是ί胃 標準差除以平均粒子直徑所得之商數的百分比。雖然對於 箸色撤粒子之形狀並無特殊限制，它們可能是肉眼視之為 球形而具有細微起伏的表面，或為非球形粒子。 根據本發明之電子攝影用調色劑是應用了上述之箸色 徼粒子。為了使此種調色劑具有適當的荷罨性質，理想的 平均粒子直徑是在3.涵1120^米，以4到15¾¾米較佳。可 使用末經修飾的箸色微粒子來作為電子攝影用調色劑。 某些添加物如調整電荷的電荷控制劑的液化劑等通常 用於一般調色劑者可適當的加入本發明之箸色微粒子中。 加入電荷控制劑的有效方法並未有特別的限制。任何 -27- (請先閲讀背面之注意事項再填窝本頁) 裝. 訂_ 本紙張尺度遑用中a B家樣毕(CNS) T4規格(210X297公*) ：0υί&gt;δ4 Λ 6 13 6 經濟部中央標準局员工消费合作社印製 五、發明説明（26) 已知可有效的用於此加入步驟的方法均可採用。例如，在 已有著色劑分散於内的聚合單體進行聚合之前加入電荷控 制劑於此聚合單體中，或以適用的電荷控制劑對箸色微粒 子進行染色之處理，令電荷控制劑快速的沈積於箸色徹粒 子的表面上。 在數値本發明之較佳具體實施例中，在生産過程中球 狀著色微粒子的内聚性或沈降作用均受到促進，而將球狀 著色微粒子自懸浮介質中固一液分離的作兩，是以在球狀 著色微粒子懸浮液中加入上述種類之水不溶性粒子來增進 之。技術上不必受限於本發明所預期的箸色撒粒子之生産 方法，而可以廣泛的運用到從懸浮介質中回收産自懸浮聚 合作用的球狀箸色微粒子，以及以固一液分離方式自主要 樹脂的微小粒子分散於水性懸浮液中（例如將樹脂組合物 在水性分散介質中加熱並溶化而形成的懸浮液）的不同分 散条統中回收微粒子。 這是由於加入水不溶性微粒子而不以待別高的溫度力Π 熱後促進了内聚或沈降作用，使得在産生的粒子圍内之球 狀著色微粒子以點接觸或越過其界面的輕微表面接觸來融 合，結果以上述普通固-液分離設備自懸浮液中分離出粒 子圍，且將分離之粒子圍乾燥並分解所得到的撤粒子。 大致上保留了自懸浮聚合中産生的微粒子之球型，且並未 顯示出任何如同使用已知的絮凝劑所産生的微粒子之顔品 質。這是因為使用相當簡單的研磨裝置、消耗能量少的分 解作用可將粒子圍變成平均粒子直徑與内聚作用前的球狀 -2&amp;- (請先閲讀背面之注意事項再填寫本頁) 裝&lt; 訂_ 線_ 本紙張尺度逍用中8 Η家標準(CNS)甲4規格(210x297公釐) 0559 Λ 6 13 6 經濟部中央楳準局员工消费合作社印製 五、發明説明（27) 著色微粒子大致相同之粒子。當然，在固-掖分離後可以 任何所需方法進行處理。例如，可採用上述生産球狀箸色 微粒子過程中之熱處理來改良徹粒子表面之性質〇咸信以 前水不溶性撤粒子作為絮凝劑，自懸浮液中回收微粒子的 技術對於生産平均粒子直徑在1到100撒米—特別是1到 5峨&amp;米的球狀微粒子特別有用，而且使得以普通離心沈降 方法將其分離或生産用於電子攝影用調色劑之球狀微粒子 (使用已知絮凝劑對其防潮性造成的破隳是一項特別嚴重 的問題）不再有困難。 在本發明之回收方法中，當加入水不溶性撤粒子以促 進懸浮液中撒粒子之内聚或沈降作m後，不需再力π熱此懸 浮液。然而若考慮到操作效率，以超過此聚合物形成所述 之球狀微粒子的Tg之溫度進行熱處理是被允許的，除非熱 處理會導致球狀微粒子的過度融合。 〈實施例〉 玆以實施例詳細說明本發明，但這些實施例僅為說明 本發明而引用，並不意味限制本發明範圍。下列實施例中 所稱「部」傜指「重量部」而言。 (實施例1 ) 在具有攪拌機，愫性氣體導入管，回流冷凝器及溫度 計之反應签，置溶有聚乙嫌醇1部之純水2, 000部，對此 加預先將過氣化$醒80部溶解於由苯乙締585部，甲基丙 嫌酸丁醋390部及甲基丙嫌酸甘油醋25部所構成b聚合甩 單體，高速攪拌使成均勻懸浮液。其次，在通氣氣下加熱 -29 ~ (請先閲讀背面之注意事項再填窝本頁) t ίτ 象 本紙張尺度遑用中國國家標準(CNS)甲4規格(210X297公龙) 05½ &lt;* Λ6 B6 經濟部中央標準局员工消費合作社印製 五、發明説明（26) 至80T：,保持此溫度繼缅擬拌5小時進行聚合，除掉水而 得以琛氣基為反應基的聚合物。 用力Π壓煉合機，將上述聚合物400部，炭黑（三菱化 學工業公司製，商品名「Carbon Black MA-100R」150部 及調整劑（保土谷化學工業公司製，商品名「Aizen Spil on Black RH」）50部煉合，在160t及100 rpm條件下 反應。冷卻後粉碎即得炭黑移植聚合物箸色劑。 在同一反應签，S溶有十二院苯礎酸銷5部之純水 8,970部。將預先以上述拔黑移植聚合物500部，偶氮雙 異丁燃_30部，2,2’—偶氮-雙—（2,4-二甲基戊_) 30音13及以苯乙嫌800部，丙嫌酸正丁醋200部及二乙締基 苯0.03部組成之混合物加入反應釜，以混合機（特殊器化 工業製，商品名「Τ·Κ· Homomixer」）以8, 000 rpmi覺株5 分，製得均勻懸浮液。 然後在通氮氣下加熱至65eC ,在此溫度繼缅攪拌5小 時進行聚合，然後再在75T：加熱1小時製得超細球狀箸色 物懸浮物（1),其變換率95.0%,平均粒度5.82wm,粒 度變異像數20. 5%。將此微球狀著色物懸浮液（1)保持於 75Π,加甲醇2*095部加熱1小時.即得粒子互相熔融的 塊狀物。過濾分離此塊狀物，以熱風乾燥機在50=0乾燥10 小時即得塊狀物1,500部，其粒子表面有局部溶融，容積 密度0.20g/ct^外觀類似麥芽膠粘製之粟子。將此塊狀 物以15kg/hr速度加進超音波噴射顆粒機（日本氣動工業 公司製，産品代號「IDS2型」）粉碎製得微細箸色物（1) -30- (請先閲讀背面之注意事项再填窝本頁) 裝. 訂- 線&lt; 本紙張尺度逍用中a國家接毕(CNS)甲4規格(210X297公*) 經濟部中央標準局员工消t合作社印製 ：0559&lt;i Λ6 _ 136_ 五、發明説明（2S) Ο 侬Coulter計數機孔徑100Wm)測定結果.該撤細 著色物的平均粒徑為5*67um,粒徑變異偽數18·7%。此 徹細箸色物（1)直接可做靜電影印機（理光公司製，代號 厂 Type 4060」）之影像産生用電子照相調色劑〇)。結 果如表1。 (實施例2) 用實施例1所用反應釜，置溶有聚乙烯醇（倉麗公司 製，代號「PVA 205」）30部之純水8, 970部。對此水，加 預先以Brill iant Carmine 6B (野間化學公司製）50部， 偶気―雙—異丁燦鳴30部及2,2’—厲気—雙—（2,4- = 甲基戊濟）30部，以及由苯乙嫌800部，丙嫌酸正丁醋200 部所組成的混合物，以混合機（特殊機工工業製，商品名 「.Τ·Κ· Homomixer」）在6,000 rpm搜伴5分製得均勾懸 浮液。 其次，將此懸浮液在通氮氣下加熱至65T：,在此溫度 繼續力卩熱5小時進行懸浮聚合，然後在751C力Π熱1小時製 得變換率98.0%,平均粒徑6·42um,粒徑變異偽數21·3 %之徽細球狀箸色粒之懸浮液（2),將此懸浮液（2)保持方$： 75它，加水性擬狀調整齊 11 (念主成分35%,東洋化學工業 製，商品名「Bontron S-34」）13部，在95Τ；力Π熱1小時 ，製得各粒子互相膝融之塊狀物。過據分取塊狀物，用減 壓乾燥機在50°C乾燥 8小時製得塊狀物1,110部，其粒子 表面局部互相結合，容積密度0· 28g/oi外觀似麥芽膠粘 -31 - (請先閲讀背面之注意事項再填窝本頁} 本紙5fc尺度逍用中8困家標準(CNS)甲4規格(210x297公龙) Λ 6 Β6 經濟部中央搮率局負工消费合作社印製 五、發明説明（30) 粟子狀。此塊狀物以12kg/hr速度供應於超音波噴射粉碎 機（日本氣動工業公司製，代號「IDS2 Type」）粉碎製 得徹細著色物⑵。 依Coulter計數器（孔100am)測定結果，此撤細 箸色微色物（2)之平均粒徑為6· 15wm,粒徑變異偽數 23· 0%。ώ微細箸色物（2)直接用於靜電影印機（理光公 司製，代號「Type 4060」）之影像産生用電子照相調色 劑（2),結果如表1。 (實施例3 ) 依實施例1之步驟製得之環須;活性基聚合物200部與 粉狀磁性材料（鈦工業公司製，商品名「Mapico Bh-200 」）400 部，用力煉合機在160T：, 100 rpm煉合，冷 卻後粉碎製得聚合物處理磁性材料。 在實施例1所用反應釜内置含陰離子表面活性劑十二 院苯礎酸鈉 5部之純水8, 970部。對此水力Π預先以上述聚 合物處理磁性材料700部，偶気-雙-異丁嫌搞30^及由 苯乙燃 800部，丙嫌酸正丁酯20Θ部及二乙嫌基苯0.1部 所構成之聚合用單體混合物，以混合機（特殊機槭化工業 公司製，商品名「T.K· Homomixer」，在8,000 rpm擬拌 5分製得均勻懸浮液。 其次，在通気氣下將此懸浮液力Π熱於651C,保持此溫 度繼續搜拌5小時實施懸浮聚合，然後加熱於75¾ 1小時 ，製得變換率98.0%，平均粒徑5.43 ym,粒徑變異偽數 22· 5%之微細球狀箸色物之懸浮液（3)。將此懸浮物（3)保 ~32 _ (請先閲讀背面之注意事項再填窝本頁) 裝- 訂· 線· 7紙張尺度逍用中a B家楳準(CNS)甲4規格(210x297公：¢) 205594 66 ΛΒ 經濟部中央櫺準局貝工消费合作社印製 五、發明説明（31) 持於75°C ,加主成分含置35%之水性漿狀調整劑41部及主 成分含量5%之氯化鋁5部，在951C處理3分製得各粒互 相熔合之塊狀物。過濾分離塊狀物，用減壓乾燥機在50T： 乾燥S小時，製得塊狀物1,700部，偽各粒子表面互相局 部熔合，容積密度0.22g/ci^,外觀類似濃稠麥芽膠粘粟 子狀。將此塊狀物以18kg/hr速度供應於超音波噴射粉碎 機粉碑製得微細箸色物⑶。 經Coulter計數器（孔100wm)測定結果，該微細 箸色物（3)之平均粒徑為5.24,粒徑變異偽數19.8%。該 微細箸色物（3)直接用於靜電影印機（佳能公司製，商品 名NP-5000)之影像産生思電子照相調色劑。結果如表1 〇 (賨施例4) 侬實施例1之步驟製得之炭黑移植聚合物，置含有陰 離子界面活性劑（第一製藥公司製，商品名「Hitenol N-08」）10部的純水於同一反應釜，對此加預先配製之坺黑 移植聚合物500部，偶気雙異丁20部，丙烯酸正丁酯 150 部，及聚丁二嫌（日本曹達公司製，商品名「Nisso -PB-B-3000」）50部之混合物，如實施例1處理得徽細球 形粒子懸浮液（4),其變換率為92%,平均粒徑6.30am 及粒徑變異像數19. 5%。 將此微細球形著色物懸浮物加熱於2小時刖得熔 合粒子之塊狀物。過濾分離塊狀物，以熱風乾燥機乾燥10 小時，製得塊狀物1,500部，其表面局部熔合，容積密度 -33- (請先閲讀背面之注意事項再填寫本頁) 本紙張尺度遑用中8國家標準(CNS)甲4規格(210X297公龙) 05594 Λ 6 136 經濟部中央楳準局兵工消费合作社印製 五、發明説明（32) 0.31k«/cn?,外觀類似濃稠麥芽膠粘粟子狀。將此塊狀物 以17k«/hr之速度供應於超音波噴射粉碎機粉碎製得微細 箸色物⑷。 依Coulter'計數器（孔100Wm)測定結果，該撒細 著色物之平均粒徑為6· 14um,粒徑變異偽數20·8%。此 撤細箸色物（4)直接用於靜電影印機（理光公司製，代號 「Type 4060」）之影像産生用電子照相調色劑。結果如 \ 表1 〇 (實施例5 ) 用實施例1所用反應器，置含有陰離子界面活性劑十 二院苯礎酸鈉 5部之純水8, 970部。蔚此加預先調配之由 烘黑移植聚合物500部，偶氡雙異丁烯%30§|5, 2,2’-偶 Μ雙-（2,4-二甲基戊30部以及苯乙燃 800部和丙 烯酸正丁醋所組成之聚合用單體製成之混合物，在混合機 中以8,000 rpni攪拌5分製成均勻懸浮液。 其次，在氮氣下將此懸浮液加熱於S5°C,保持此溫度 繼續攪拌5小時進行懸浮聚合，然後加熱於75Ό 1小時， 製得變換率95.0%,平均粒徑5.92um,粒徑變異像數 23. 0%之微細球形著色物懸浮液（5)。將此懸浮掖（5)保 持於751〇,力Π1Ν鹽酸200部，加熱於85t三小時，製得熔 合粒子之塊狀物。過據分離此塊狀物，用減壓乾燥機在50 X：乾燥 8小時，得塊狀物1,500部，其粒子表面傜局部熔 合，容積密度0.35g/cm3，外觀類似濃稠麥芽膠粘住粟子 狀。將此塊狀物以13kg/hr之速度供應於超音波噴射粉碎 -34- (請先閲讀背面之注意事項再填窝本頁) 本紙張尺度逍用中B國家楳準(CNS)甲4規格(210X297公釐) 05594 經濟部中央標準局β工消費合作社印製 五、發明説明（33) 機粉碎製得微細著色物(5) 0 依Coulter計數器（孔100ym)測定結果，該微細 箸色物（5)的平均粒徑5.65 w m ,粒徑變異偽數21 · 2%。 該撒細箸色物（5)直接用於靜電影印機（理光公司製，厂 Type 4060」）之影像産生用電子照相調色劑。結果如表 1 〇 (實施例6) 侬實施例4之步驟，但以氛磺化聚乙烯（杜邦公司製 ,商品名「HypoIon 20」）50部取代聚丁二-蹄50咅15,並以 過氣化苯醯30部取代偶氮雙異丁烯％ 20部及2, 2 ^ _偶気雙 (2,4-二甲基戊鳴）10部，製得變換率92^，平均粒徑 6· 02 xz m ,粒徑變異偽數21 · 2%之微細球狀箸色物之懸浮 液（6)。將此懸浮液（S)保持於75¾，力Π氛化鈴S部，在 95T：加熱1小時製得熔合粒子之塊狀物。過濾分離此塊狀 物，用減壓乾燥機在501乾燥8小時，製得各粒子表面局 部熔合，容積密度0.21g/euA外觀類似濃麥芽膠粘住粟 子狀之塊狀物1,500部。此塊狀物以18kg/hr速度供應超 音速噴射粉碎機粉碎製得微細箸色物（6)。 經Coulter計數器（孔100測定結果，該箸色 物（&amp;)之平均粒徑為6.10wm,粒徑變異偽數22.0%。此 微細箸色物（6)直接用於靜電影印機（理光公司製，「 Type 4060」）之影像産生用電子照相調色劑。結果如表 1 〇 (實施例7 ) - -35- (請先閲讀背面之注意事項再蜞窝本頁) 裝- 訂- 本紙張疋度逍用中國a家樣準(CNS)甲4規格(210x297公*) 05594 Λ 6 136 經濟部中央標準局貝工消費合作社印製 五、發明説明（己4) 依實施例1之步驟，但以非離子界面活性劑（三徉化 成公司製，商品名「Nonipoi 200」）10部取代十二院苯 礎酸鈉5部，製得變換率96%,平均粒徑5.75^111,粒徑 變異傺數19. 5%之微細球狀箸色物懸浮液（7)。將此懸浮 液（7)保持於60T：,加已院 750部，加熱1小時製得焰合 粒子塊狀物。過濾分離此塊狀物，用熱風乾燥機在5010乾 燥10小時，得粒子表面局部溶合•容積密度0*22g/cnA 外觀類似粘稠麥芽膠粘粟子狀之塊狀物1,500部。將此塊 狀物以15ks/hr速度供給於超音波噴射粉碎機粉碎製得微 細著色物（7)。 經Coulter計數器（孔100wm)測定結果，該微細 箸色物之平均粒徑為S.SSwrn,粒徑變異偽數0.7%。此 微細著色物（7)直接甩於靜電影印機（理光公司製，「NP 4060」）之影像産生用調色劑。結果如表1。 (實施例8) 侬零施例1製得微細球狀箸色物之懸浮液（1),此懸 浮物（1)保持於75°C ,與預先配製之純水1, 000部中分散導 電性坺黑（¾水指數12*3, Ketjen國際公司製，商品名「 Ketjen EC」）10部之分散液500部混合，加熱1小時則 得粒子熔合之塊狀物，過濾分離此塊狀物，用熱風乾燥器 在50C乾燥10小時，製得粒子表面局部熔合，容積密度 0.18g/cm3,外觀類似麥芽膠粘位栗子狀之塊狀物 1,500 部。將此塊狀物以16kg/hr速度供給於超音波噴射粉碎 ，機粉碎製得微細著色物（8)。 -36- (請先閲讀背面之注意事項再填寫本頁) 裝- 訂- -線&lt; 本紙張尺本遑用中B 8家揉準(CHS)甲4規格(210x297公逢) 05594 經濟部中央標準局貝工消脅合作社印製 五、發明説明（35) 經Coulter計數器（孔100“ m)測定結果，該微細 著色物（8)之平均粒徑為5· 78 w m ,粒徑變異偽數17·5% 。此微細箸色物（S)直接用於靜電影印機（理光公司製， 「Type 4060」）之影像産生用電子照相調色劑。結果如 表1 〇 (實施例9) 依實施例8之步驟，但Ketjen EC之水性分散液500 部改為預先以if水性微砂粉（_水指數50· 5，日本徹砂製） 10部，導電性度黑（殊水指數12.3，KetJen國際公司製， 商品名「Ketjen EC」）5 部分散於甲醇150部之分散液 123. 8部，加熱1.5小時，製得粒子塊。過濾分離塊狀物， 用減壓乾燥機在50°C乾燥8小時，得塊狀物1500部，其粒 子表面偽局部溶合，容積密度0*17g/enA外觀類似濃麥 芽願粘住粟子狀。這些塊狀物以20kg/hr速度供給於超音 波噴射粉碎機粉碎製得撒細箸色物（9)。 此著色物（9)經Coulter計數器（孔100wm)測定 ,其平均粒徑為5.81am,粒徑變異傜數17· 1 %。此微 細著色物（9)直接用於靜電影印機（佳能公司製，「NP -5000」）之影像産生用調色劑。結果如表1。 (實施例10) 侬實施例2製得微細球狀箸色物之懸浮液（2),將此 懸浮液保持於751〇,加預先以水性漿狀調整劑（含主成分 35%，東浑化學公司製，商品名「Bontron S-34」）13部 及性微δ夕粉RQ72 (日本微砂公司製）10部分散於甲醇 -37 - {請先閲讀背面之注意事項再填窝本頁} 本紙張尺本遑用中Β Β家猱準(CNS)甲4規格(210x297公*)This paper is used in the S 8 Standards (CfNS) A4 specifications (2 丨 0x297 g). Printed by the Central Economic Department of the Ministry of Economic Affairs. Cooperative cooperative Λ 6 ______J36_ V. Description of the invention (20) Material blue Setan, Victorian Blue Temple, Aura Blue, Non-Metallic Mood Blue, Partial Atomization of Phthalodon Blue, Fast Sky Blue and #Man Blue BC, as well as green pigments such as% color B, Peacock thread color hall and Fana Seoul (Fanal) yellow crepe G and so on. Charge control agents that can be effectively used in the present invention include aniline, monoazo dyes, boll, cetyl hexanoate, alkyl esters of% formic acid, and arylamides, nitrohumic acid, Ν, Ν- Metal powders of tetrashenyldiamine dibenzyl copper, N, N-tetramethylbenzidine, trityq, and salicylic acid are known as charge control agents in the field of electrophotography. Insects that can be effectively used in the present invention include polymer powders with a Chen-shaped softening point ranging from 80 r: to: LSO r, high-yielding stone clams with a melting point of 70 ° C to 60 C, and fatty acid esters And its partially saponified derivatives, high fatty acids, metal salts of fatty acids, and higher alcohols. Inorganic powders that can be effectively used in the present invention include aluminum, titanium dioxide, titanium titanate, titanium titanate, calcium titanate, total acid, gasified fresh, silica sand, clay, mica, flat spar, Silica, various inorganic gasification tree pigments, chromium dichloride, sulphur dioxide, iron red, antimony gasification, gasification sieve, gasification error, barium sulfate, methacrylic acid, acid cracking, sand, nitrification The neutrinos or grains of silicon, nitrided sand, boron sulfonate, tungsten master, titanium master and black. Among the water-insoluble powders mentioned above, those with a hydrophobicity index (Mν /: methanol concentration) of 5 or more are particularly desirable, because they can impart ideal moisture resistance to spherical emblem particles prepared by decomposition. When spherical microparticles are used as electrophotographic rain toners, they are also shown to contribute to charge stability. The above particularly suitable water-insoluble powders include a variety of inorganic chlorides such as sand, titanium, and sharp, which have been processed to distinguish between black and black (Ketjen) -22- &lt; Please read the precautions on the back before filling this page) Installed &lt; The printed paper Λ scale side is used in the aa family of “CNS” TM specifications (210X297 g; ¢) Λ 6 Β6 Printed by Beigong Consumer Cooperative of Central Bureau of Standards of the Ministry of Economy V. Description of invention (2Π) Black, acetylene ink He Fury's hydrophobic and conductive types. The term "hydrophobic index" used in this article refers to the value obtained in the following steps. (1) Put 0.2g of the given sample in a 200ml beaker and dilute with 50ml of pure water. (2) Continuously stir the sample aqueous solution with a magnetic stirrer, and add methanol under the surface of the carrying solution. (S) The moment when the sample is not visible on the surface of the stirring pan is regarded as the final black test. (4) Calculate the sample water content based on the amount of methanol consumed in the test according to the following equation. Hydrophobicity index (%) = [X / (50 + X)} X100 where X represents the amount of methanol (ml). In view of the charge stability of the toner with a small particle diameter required to produce high resolution, the water-insoluble fine particles selected in the present invention need to have electrical conductivity. The conductive water-insoluble fine particles that can be effectively used in the present invention include conductive black powder, titanium dioxide and vaporized tin plus gasification, conductive powdered vaporized gold and black powder. In order to effectively achieve the above goals, the particle diameter of such water-insoluble particles must be between 0.001 and 10 microns, preferably between 0.005 and 5 particles. If the particle diameter of the water-insoluble emblem particles does not exceed 0.001 emblem. It may cause the effect of adding these particles, that is, significantly improve the flocculation properties, decomposability, fluidity, scavenging, etc. When the colored particles are used as electrons The characteristics that can be exhibited in photographic toners no longer appear. On the contrary-2 counseling-(please read the precautions on the back before filling in the nest page) 装 ·-线-This paper is used in China National Standard A (CNS) A 4 specifications (210 &gt; &lt; 297 public goods ) 5. Description of the invention (22) Printed by the Beigong Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. If the particle diameter of the water-insoluble fine particles exceeds 10 microns, the effect of adding these particles may be very low, and the particles will be removed when the color is The improvement in resolution that should be produced when used as a toner for electrophotography does not occur. The selection of the amount of additive force for these water-insoluble microparticles is quite wide, depending on the type of water-insoluble microparticles used and the particle diameter. If the child is very small, it is difficult to add these particles to show the effect. If the amount is very large, when the color emblem particles are used as toners for electrophotography, there may be side effects in terms of charge properties and environmental stability. Therefore, the amount of the additive is preferably in the range of 0.01 to 10 by weight, and the range of 0.1 to U 50 parts by weight is the best-the polymerized monomer composition is 100 parts by weight. The various water-insoluble pellets mentioned above can be used alone or in a mixture of two or more to be shaken. Needless to say, even when water-insoluble microparticles are used, the above-mentioned known flocculant or mole solvent can also be used to produce spherical colored microparticles, unless combined use will cause inconvenience. Generally, it is possible to add an appropriate organic solvent to Promote integration. Due to the cohesion or sedimentation of spherical colored microparticles caused by the addition of water-insoluble microparticles of the above type into an aqueous suspension, this additive is added to the suspension of spherical microparticles and the resulting mixture in It is produced by placing it for a specified period of time without additional heating. In the method for producing colored microparticles of the present invention, there is no problem with supplying the heat source within the specified range, because the spherical colored emblem particles generated from the suspension polymerization have become in a state of fusion with each other, especially when the particles are fused with each other and they lose all The status of the interface. Specifically, when the suspension of the spherical colored particles is heated by the first method described above to perform the fusion of spherical colored particles-24-(please read the precautions on the back before filling this page) This paper The standard BB family «Bi (CNS &gt; T4 specification (210x297 g *)) Λ 6 Β6 Printed by the Ministry of Economic Affairs Central Standards Bureau Ordnance Industry Cooperative V. Inventive notes (23) During the heat treatment, water-insoluble fine particles can be added After heating at a temperature in the range of 501C to 130T: the spherical crimson colored particles are cohesive so that the fusion is thrown, and they can continue to develop. Limulus is taken from the suspension medium as the second or third method above. When the spherical cinder-colored pellets are subjected to heat treatment to fuse the spherical cinder-colored fine particles, the force can be heated at a temperature within the range of 50 ^: to 130 r: or less, within The state of fusion in the bulk agglomerates of the suspension reaches a certain degree. In the above first method, the heat treatment method for fusing spherical celebrity particles is to heat the suspension force, in this case from the suspension Obtained by the fusion of spherical colored emblem particles The way of particle encirclement is to use ordinary solid-liquid separation device-using the principle of suction filtration, pressure filtration or centrifugal filtration. The fusion state generated in the particle encirclement is best to make the fusion product have 0.1-1 to 0.9 The bulk density of grams / cubic centimeter is 0 · Timber * 7 grams / cubic centimeter. Although the shape or size of the particle garden is not limited, it is best to form particles with an average size of 20 to 10,000 particles. The particle size is 30 to 1,000, and it is the best. It is considered to facilitate the work of totalization, drying and decomposition after the thermal fusion process. If the size is less than 20 microns, the particle recovery needs to consume very large Energy or special equipment. If its size exceeds 10,000 emblems, decomposition requires huge energy. The particle garden obtained from the above will then go through the drying step to the decomposition step. In the above second and first In the three methods, in order to fuse spherical custody particles, heat treatment is carried out on the spherical colored particles taken from the suspension medium. It is best to cohere the spherical custody particles into cohesive particles, thinking that After that, the spherical colored particles are separated from the suspension medium for preparation, -25- (please read the precautions on the back and then fill out this page) Binding-Order-Line-This paper size is selected using the Chinese Standard (CNS) A 4 specifications (210x297 gongs) Λ 6 13 6 Printed by the Beigong Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs V. Description of invention (24) This is helpful for separation with ordinary solid-liquid separation equipment. The skull density is preferably in the range of 0.05 to 0.9 grams / cubic centimeter, and the best is 0.1 to 0.7 grams / cubic centimeter. Although the shape and size of the particle aggregates are not limited, they are best It is better to generate particles with an average size of 11 10,000 microns in 2 culverts, preferably 30 to 1,00ΘΜ meters. This is to facilitate the reduction, drying, and decomposition work after thermal fusion treatment. In these methods, the heat treatment described above is performed on the spherical colored microparticle blocks recovered as described above, and as a result, a particle garden formed by the fusion of spherical dust-like microparticles is obtained. The state of fusion is preferably such that the particle circumference has a volume density of 1 to 0.9 g / cm3, and the best is 0 · 2®Ι0 · 7 g / cm3. As in the first mode described above, the particle garden proceeds to the decomposition step through the drying step. In the decomposition step, the particle circle in the dry state is decomposed into spherical dust-like microparticles having an average particle diameter approximately the same as before fusion. Any industrially produced grinding equipment that has been used as granules and granules can be used for decomposition. In an ideal way, the effect of decomposing into an average particle diameter that is approximately equal to the spherical celebrity microparticles before fusion (as listed in this article for reference) has the ability to make individual particles in the particle garden of self-fused spherical celebrity microparticles The degree to which the unfinished gold loses its interface (as clearly shown in the electron scanning photomicrograph at magnification in Figure 1), is decomposed into spherical spherical color withdrawal particles before the fusion, resulting in particles in the surroundings of each particle It returns to the state where the spherical colored fine particles only deform before decomposition. However, it is indeed difficult to control to make the interface fusion state uniform. As clearly shown in the 2IM electron scanning microphotograph (1500 times), the color-removing particles to be manufactured are usually emblem particles. -26- (please read the precautions on the back before writing this page) Order · Line &lt; This paper standard is easy to use and sleepy Η family standard (CNS) A 4 specifications (210X297 mm) 1.0559 ^ Λ 6 Β6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention description (25) Mixture Formed, this mixture is produced by the spherical colored particles deforming and breaking before fusion and decomposition, and the broken K is attached to the deformed particles. Even when a batch of colored microparticles is a mixture of the above, their quality is never worse than that of ideal type microparticles, as long as the average particle diameter of the spherical colored microparticle mixture is approximately the same as the spherical colored microparticles before fusion and decomposition. In this example, when the rate of change of the average particle diameter of the crimson colored microparticles is within 20% of the spherical clamshell colored particles (preferably within 10¾, more preferably within 5%), the colored microparticles and spherical The average particle diameter of the celebrity microparticles can be regarded as approximately the same. The distribution of the particle diameter and the particle diameter of the color-retracting particles produced by the above method has been controlled as required. However, the ideal particle diameter range is between 115 and 5 metres of culverts, with 3.20 U20 sami as the best, and the distribution of the average particle diameter is such that the variation of the particle diameter is within the range of 0 to 80 ^ to sleep 1150% is better. The term "particle diameter variation pseudo-number" here is the percentage of the quotient obtained by dividing the standard deviation of the stomach by the average particle diameter. Although there is no particular restriction on the shape of the cyan particles, they may be regarded as spherical with a slightly undulating surface by the naked eye, or they may be non-spherical particles. The toner for electrophotography according to the present invention employs the above-mentioned color toner particles. In order to make this toner have proper charge properties, the ideal average particle diameter is 3.120 mm, preferably 4 to 15 mm. As the toner for electrophotography, unmodified celebrity colored microparticles can be used. Certain additives such as liquefaction agents for charge control agents that adjust charge are generally used in general toners and can be appropriately added to the microparticles of the present invention. The effective method of adding a charge control agent is not particularly limited. Any-27- (please read the precautions on the back before filling in the nest page). Binding. This paper size is used in a B home sample (CNS) T4 specification (210X297 g *): 0υί &gt; δ4 Λ 6 13 6 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 5. Description of Invention (26) Any method known to be effective for this joining step can be used. For example, adding a charge control agent to the polymerized monomer before polymerizing the polymerized monomer in which the existing colorant is dispersed, or dyeing the colored microparticles with a suitable charge control agent, so that the charge control agent quickly It is deposited on the surface of the cerise particles. In several preferred embodiments of the present invention, the cohesiveness or sedimentation of the spherical colored microparticles is promoted during the production process, and the solid-liquid separation of the spherical colored microparticles from the suspension medium is performed in two, It is improved by adding water-insoluble particles of the above kind to the suspension of spherical colored microparticles. Technically, it is not necessarily limited to the production method of the custody dust particles expected by the present invention, but can be widely used to recover the spherical custody fine particles produced by suspension polymerization from the suspension medium, as well as the solid-liquid separation method. The fine particles of the main resin are dispersed in an aqueous suspension (for example, a suspension formed by heating and dissolving the resin composition in an aqueous dispersion medium) to recover fine particles. This is due to the addition of water-insoluble microparticles without waiting for another high temperature force Π after heating to promote cohesion or sedimentation, so that the spherical colored microparticles within the generated particles are in point contact or a slight surface contact across their interface In order to achieve fusion, as a result, the surrounding particles are separated from the suspension by the above-mentioned ordinary solid-liquid separation equipment, and the separated particles are dried and decomposed to obtain the withdrawn particles. The spherical shape of the microparticles produced from suspension polymerization is substantially retained, and does not show any quality of the microparticles as produced using known flocculants. This is because the use of a relatively simple grinding device and a decomposition effect that consumes little energy can turn the particles into a spherical shape before the average particle diameter and cohesion -2 (Please read the precautions on the back before filling in this page) &lt; 訂 _ 線 _ This paper is used in the 8 standards of the family standard (CNS) A 4 specifications (210x297 mm) 0559 Λ 6 13 6 Printed by the Employee Consumer Cooperative of the Central Department of Economics, Ministry of Economic Affairs V. Invention Instructions (27) Particles with roughly the same coloration. Of course, after solid-nye separation, it can be treated in any desired way. For example, the heat treatment in the process of producing spherical dust particles can be used to improve the properties of the surface of the particles. Xianxin previously used water-insoluble particles as a flocculant, and the technology of recovering particles from the suspension for the production of average particle diameters from 1 to 100 Sami—especially spherical particles of 1 to 5 Angstroms &amp; meters are particularly useful, and make them separated by ordinary centrifugal sedimentation methods or produce spherical particles for toners for electrophotography (using known flocculants) The breaking of the barrier caused by its moisture resistance is a particularly serious problem) no longer has difficulty. In the recovery method of the present invention, when water-insoluble particles are added to promote the cohesion or settling of particles in the suspension, it is not necessary to heat the suspension again. However, if the operating efficiency is taken into consideration, heat treatment at a temperature exceeding the Tg of the polymer to form the spherical fine particles is allowed unless the heat treatment causes excessive fusion of the spherical fine particles. <Examples> The present invention is described in detail with examples, but these examples are cited only for illustrating the present invention and are not meant to limit the scope of the present invention. In the following examples, the term "part" refers to the "weight part". (Example 1) In a reaction tag equipped with a stirrer, a gas introducing tube, a reflux condenser and a thermometer, 2,000 parts of pure water in which 1 part of polyethylene glycol is dissolved are added, and this is pre-gasified $ Dissolve 80 parts in 585 parts of styrene, 390 parts of methyl propionate butyrate and 25 parts of methyl propionate glyceride. B Polymerize the monomer and stir at high speed to make it into a uniform suspension. Secondly, heat under ventilation -29 ~ (please read the precautions on the back before filling the nest page) t ίτ The size of the paper is based on the Chinese National Standard (CNS) A4 specification (210X297 male dragon) 05½ &lt; * Λ6 B6 Printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Invention description (26) to 80T: Maintain this temperature and continue to mix for 5 hours for polymerization, remove the water to obtain a gas-based polymer. Using a forceful Π kneading machine, combine the above 400 polymers, carbon black (manufactured by Mitsubishi Chemical Industries, Ltd., trade name "Carbon Black MA-100R" 150) and modifier (manufactured by Hodogaya Chemical Industries Co., Ltd., trade name "Aizen Spil" "On Black RH") 50 parts are mixed and reacted under the conditions of 160t and 100 rpm. After cooling, it is crushed to obtain the carbon black graft polymer pigment. In the same reaction, S dissolves 5 parts of twelve benzoic acid. 8,970 parts of pure water. 500 parts of the above-mentioned black polymer will be transplanted in advance, 30 parts of azobisisobutane burning, 2,2'-azo-bis- (2,4-dimethylpentane) 30 Tone 13 and a mixture consisting of 800 parts of styrene and ethyl, 200 parts of n-butyric acid propionate and 0.03 of diethylbenzylbenzene are added to the reaction kettle, and a mixer (manufactured by special chemical industry, trade name "Τ · Κ ·" Homomixer ”) 5 minutes at 8,000 rpm to prepare a homogeneous suspension. Then heated to 65eC under nitrogen, followed by polymerization at this temperature for 5 hours, followed by polymerization at 75T: heating for 1 hour Fine spherical suspended solids (1), its conversion rate is 95.0%, the average particle size is 5.82wm, and the particle size variation is 20.5%. This microsphere The coloring matter suspension (1) is kept at 75Π, plus methanol 2 * 095 part and heated for 1 hour. That is, a mass of particles melting with each other. The mass is filtered and separated, and dried with a hot air dryer at 50 = 0 for 10 hours. A mass of 1,500 pieces was obtained, and the surface of the particles was partially melted, and the bulk density was 0.20g / ct ^. The appearance was similar to the millet made of malt glue. This mass was added to an ultrasonic jet particle machine at a speed of 15kg / hr (Japan Made by Pneumatic Industry Co., Ltd., product code "IDS2") crushed to produce fine chopsticks (1) -30- (please read the precautions on the back before filling the nest page). Binding-Line &lt; This paper size Printed in China National Standards (CNS) Grade A (210X297) * Printed by the Ministry of Economic Affairs, Central Standards Bureau, Employee Consumer Cooperative: 0559 &lt; i Λ6 _ 136_ V. Description of Invention (2S) Ο Non-Coulter Counter Aperture 100Wm) Results of the measurement. The average particle size of the finely drawn coloring matter was 5 * 67um, and the pseudo-number of particle size variation was 18.7%. This thorough color (1) can be directly used as an electrophotographic toner for image production of a static film printer (manufactured by Ricoh Co., Ltd. Type 4060)). The results are shown in Table 1. (Example 2) In the reaction kettle used in Example 1, 30, 970 parts of pure water in which 30 parts of polyvinyl alcohol (manufactured by Cangli Company, codenamed "PVA 205") were dissolved. For this water, add 50 units of Brill iant Carmine 6B (manufactured by Noma Chemical Co., Ltd.) in advance, 30 units of Ochi-shuang-isoding Canming and 2,2'-Li-Shuang- (2,4- = methylpentyl ) 30 parts, and a mixture consisting of 800 parts of styrene and 200 parts of n-butyric acid propionate, searched at 6,000 rpm with a mixer (manufactured by special machinery industry, trade name ".Τ · Κ · Homomixer") 5 minutes to prepare a suspension of all hooks. Secondly, the suspension was heated to 65T under nitrogen: Continue to heat at this temperature for 5 hours for suspension polymerization, and then heat at 751C for 1 hour to obtain a conversion rate of 98.0%, an average particle size of 6.42um, The particle size variation pseudo number is 21.3%, the suspension of fine spherical spherical colored particles (2), keep this suspension (2) Fang $: 75 it, add water-like pseudo-like adjustment Qi 11 (main ingredient 35 %, Manufactured by Toyo Chemical Industries, trade name "Bontron S-34"), 13 parts, at 95T; heated for 1 hour, to make a lump of particles melted with each other. The blocks were collected according to the data, and dried in a vacuum dryer at 50 ° C for 8 hours to obtain 1,110 blocks. The surface of the particles was partially combined with each other, and the bulk density was 0.28g / oi. -(Please read the precautions on the back before filling in the nest page) This paper is 5fc standard for easy use, 8 sleepy home standards (CNS), A 4 specifications (210x297 male dragons) Λ 6 Β6 Printed by the Consumer Labor Cooperative of the Central Bureau of the Ministry of Economic Affairs System V. Description of the invention (30) Millet shape. This lump is supplied to an ultrasonic jet mill (manufactured by Japan Pneumatic Industry Co., Ltd., codenamed "IDS2 Type") at a speed of 12 kg / hr to obtain a finely colored product. ⑵ Coulter counter (hole 100am) measurement results, the average particle size of this fine dust-colored fine color material (2) is 6.15wm, and the particle size variation pseudo number is 23.0%. The fine fine dust-colored material (2) is directly used for Static film printer (manufactured by Ricoh Corporation, code-named "Type 4060") electrophotographic toner (2) for image generation, the results are shown in Table 1. (Example 3) The ring must be prepared according to the steps of Example 1; activity 200 parts of base polymer and 400 parts of powdery magnetic materials (manufactured by Titanium Industries, trade name "Mapico Bh-200") , Mixed with a force mixer at 160T :, 100 rpm, cooled and pulverized to obtain a polymer-treated magnetic material. The reaction kettle used in Example 1 contains 5 parts of pure water containing anionic surfactant sodium twelve sodium benzoate 8, 970. For this hydraulic Π, 700 magnetic materials are treated with the above polymer in advance, even 30% of bismuth-bis-isobutyl is burned, and 800 are burned by styrene, 20θ of n-butyl propionate and diethyl The monomer mixture for polymerization consisting of 0.1 parts of suspected benzene was prepared with a mixer (manufactured by Special Machine Kakin Chemical Industry Co., Ltd., trade name "TK · Homomixer") at 8,000 rpm for 5 minutes to prepare a uniform suspension. Secondly, in Heat the suspension to 651C under ventilated air, keep the temperature and continue to mix for 5 hours to implement suspension polymerization, and then heat to 75¾ 1 hour, the conversion rate is 98.0%, the average particle size is 5.43 ym, the particle size variation pseudo number 22 · 5% suspension of fine spherical custard (3). Keep this suspension (3) ~ 32 _ (please read the precautions on the back before filling the nest page) Pack-Order · Thread · 7 Paper size for easy use a B Jiashu standard (CNS) A 4 specifications (210x297 g: ¢) 205594 66 ΛΒ Central Ministry of Economic Affairs Printed by Jubei Consumer Cooperative Co., Ltd. V. Description of invention (31) Hold at 75 ° C, add 41 parts of aqueous slurry regulator containing 35% of main ingredient and 5 parts of aluminum chloride with 5% of main ingredient at 951C After processing for 3 minutes, the lumps of the particles fused with each other are obtained. The lumps are separated by filtration and dried at 50T with a reduced pressure dryer for 1 hour to obtain 1,700 lumps. The surfaces of the pseudo particles are partially fused with each other and the bulk density 0.22g / ci ^, the appearance is similar to thick malt gum-like millet. This mass was supplied to the ultrasonic jet pulverizer powder at a rate of 18 kg / hr to obtain a fine custard ⑶. According to the measurement result of the Coulter counter (hole 100wm), the average particle size of the fine chopsticks (3) is 5.24, and the particle size variation pseudo-number is 19.8%. The fine chopsticks (3) are directly used in image-generating toners for image production of still-film printers (manufactured by Canon, trade name NP-5000). The results are shown in Table 10. (Carbon Example 4) The carbon black graft polymer prepared in the procedure of Example 1 contains 10 anionic surfactants (trade name "Hitenol N-08" manufactured by Daiichi Pharmaceutical Co., Ltd.). In the same reaction kettle, add 500 pre-prepared Ai black graft polymers, 20 parts of diisobutyl diisobutyl, 150 parts of n-butyl acrylate, and polybutadiene (manufactured by Soda Corporation, Japan) "Nisso -PB-B-3000") 50 parts of the mixture, treated as in Example 1 to obtain a fine spherical particle suspension (4), the conversion rate is 92%, the average particle size 6.30am and the particle size variation number 19 . 5%. This fine spherical colored substance suspension was heated for 2 hours to obtain a mass of fused particles. Filter and separate the lumps, and dry them with a hot air dryer for 10 hours to obtain 1,500 lumps, the surface of which is partially fused, and the bulk density is -33- (please read the precautions on the back before filling this page) This paper is for standard use China National Standard 8 (CNS) Grade A 4 (210X297 male dragon) 05594 Λ 6 136 Printed by the Ordnance Industry Consumer Cooperative of the Central Department of Economics of the Ministry of Economic Affairs V. Description of Invention (32) 0.31k «/ cn ?, similar in appearance to thick wheat Buds are sticky and millet-shaped. This lump is supplied to a supersonic jet mill at a speed of 17k «/ hr to obtain a fine dust-colored substance⑷. According to the measurement result of Coulter's counter (hole 100Wm), the average particle size of the fine coloring matter is 6.14um, and the particle size variation pseudo-number is 20 · 8%. This fine crimson color removal material (4) is directly used in electrophotographic toners for image generation of still film printers (manufactured by Ricoh Corporation, codenamed "Type 4060"). The results are shown in Table 1 〇 (Example 5) Using the reactor used in Example 1, 8,970 parts of pure water containing 5 parts of anionic surfactant sodium twelve sodium benzoate were placed. We add 500 pre-provisioned black-bearing graft polymers, even radon bisisobutylene% 30 § | 5, 2,2'-even M bis- (2,4-dimethylpentane 30, and styrene 800 The mixture of the monomer and the polymerization monomer composed of acrylic acid n-butyl vinegar was stirred at 8,000 rpni in the mixer for 5 minutes to make a uniform suspension. Secondly, the suspension was heated to S5 ° C under nitrogen and kept This temperature was continuously stirred for 5 hours for suspension polymerization, and then heated at 75Ό for 1 hour to prepare a fine spherical coloring substance suspension (5) with a conversion rate of 95.0%, an average particle size of 5.92um, and a particle size variation of 23.0%. Keep this suspension (5) at 7510 and 200 parts of hydrochloric acid, heated at 85t for three hours to prepare a lump of fused particles. Separate the lump according to this and use a vacuum dryer at 50 X: After drying for 8 hours, 1,500 pieces were obtained, and the surface of the particles was partially fused, the bulk density was 0.35g / cm3, and the appearance was similar to the thick malt glue sticking to the millet shape. This piece was supplied at a rate of 13kg / hr Ultrasonic Jet Crush-34- (Please read the precautions on the back before filling the nest page) This paper size is used in the country B (CNS) A4 specifications (210X297 mm) 05594 Printed by the β-Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of the invention (33) Fine coloring material obtained by machine crushing (5) 0 According to the measurement result of Coulter counter (hole 100ym) , The average particle size of the fine chopsticks (5) is 5.65 wm, and the pseudo-number of particle size variation is 21.2%. The scattered chopsticks (5) are directly used in static film printers (manufactured by Ricoh, Type 4060) ) Of the electrophotographic toner used for image generation. The results are shown in Table 1 (Example 6). The procedure of Example 4 is replaced by 50 parts of sulfonated polyethylene (manufactured by DuPont, trade name "HypoIon 20"). Polybutadiene-hoof 50 咅 15, and 30 parts of azo bisisobutylene replaced by 30 parts of azo bisacrylic acid and 10 parts of 2, 2 ^ _ 気 bis (2,4-dimethylpentamidine), prepared The conversion rate was 92 ^, the average particle size was 6.02 xz m, and the particle size variation pseudo-number was 21.2%. A suspension of fine spherical custard (6). Keep this suspension (S) at 75¾, force Π Atomized bell S part, at 95T: heating for 1 hour to prepare a lump of fused particles. The lump was separated by filtration and dried at 501 with a reduced pressure dryer for 8 hours to prepare the surface of each particle Partially fused, bulk density 0.21g / euA looks like thick malt gum and sticks to 1,500 pieces of millet-shaped pieces. This piece is supplied to a supersonic jet mill at 18kg / hr to obtain fine dust color (6 ). As measured by a Coulter counter (hole 100), the average particle size of the pigment (&amp;) is 6.10wm, and the particle size variation pseudo-number is 22.0%. This fine chopstick (6) is directly used as an electrophotographic toner for image production in a static film printer (manufactured by Ricoh Corporation, "Type 4060"). The results are shown in Table 1 〇 (Example 7)--35- (please read the precautions on the back and then slap this page) Binding-Order-This paper is used in China A standard (CNS) A4 specifications ( 210x297 public *) 05594 Λ 6 136 Printed by the Beigong Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of invention (4) Follow the steps of Example 1, but use a non-ionic surfactant (Sanyo Chemical Co., Ltd., trade name) "Nonipoi 200") 10 parts replaced 5 parts of sodium benzoate in the twelfth hospital, to obtain a fine spherical clinker suspension with a conversion rate of 96%, an average particle size of 5.75 ^ 111, and a particle size variation of 19.5% (7). Keep this suspension (7) at 60T :, add 750 units of the hospital and heat for 1 hour to prepare a mass of flame particles. The block was separated by filtration, and dried in a hot air dryer at 5010 for 10 hours. The surface of the particles was partially dissolved. The bulk density was 0 * 22g / cnA. The appearance was similar to viscous malt-glued millet-shaped blocks of 1,500 parts. This mass was supplied to an ultrasonic jet mill at a rate of 15ks / hr to pulverize to obtain a fine coloring matter (7). According to the measurement result of Coulter counter (hole 100wm), the average particle size of the fine cinder is S. SSwrn, and the particle size variation pseudo-number is 0.7%. This fine coloring matter (7) is directly thrown at the toner for image generation of a static film printer (manufactured by Ricoh Corporation, "NP 4060").结果 如 表 1。 The results are shown in Table 1. (Example 8) A suspension (1) of fine spherical cinder-colored substance prepared in Example 1 of Nongling, this suspension (1) is kept at 75 ° C, and is electrically conductively dispersed in 1,000 parts of pure water prepared in advance Sexual blackness (¾ water index 12 * 3, manufactured by Ketjen International Co., Ltd., trade name "Ketjen EC"), 500 parts of 10 dispersions are mixed, heated for 1 hour to obtain a lump of particle fusion, and the lump is filtered and separated And dried with hot air dryer at 50C for 10 hours, the surface of the prepared particles was partially fused, the bulk density was 0.18g / cm3, and the appearance was similar to the 1,500 pieces of chestnut-shaped lump with malt adhesive position. This lump was supplied to ultrasonic jet crushing at a rate of 16 kg / hr, and was crushed by a machine to obtain a fine colored substance (8). -36- (Please read the precautions on the back before filling in this page) Binding- Order- -Line &lt; This paper ruler is used in the B 8 home churn (CHS) A 4 specifications (210x297 public meeting) 05594 Ministry of Economic Affairs Printed by the Beigong Xiaowen Cooperative of the Central Bureau of Standards 5. Description of the invention (35) As measured by a Coulter counter (hole 100 ”m), the average particle size of the fine colored substance (8) is 5.78 wm, and the particle size variation is pseudo The number is 17 · 5%. This fine chopstick (S) is directly used in electrophotographic toner for image production of static film printer (manufactured by Ricoh Corporation, "Type 4060"). The results are shown in Table 1 〇 (Example 9) The procedure of Example 8 was followed, but 500 parts of the aqueous dispersion of Ketjen EC were changed to 10 parts of water-based micro-sand powder (water index 50 · 5, made by Japan Toshisha) in advance. , The conductivity is black (special water index 12.3, manufactured by KetJen International Corporation, trade name "Ketjen EC") 5 parts are dispersed in 150 parts of methanol, 123.8 parts of the dispersion liquid, heated for 1.5 hours to obtain a particle block. Separate the lump by filtration and dry it at 50 ° C for 8 hours with a reduced pressure dryer to obtain 1500 lump. The surface of the particles is pseudo-partially dissolved. The bulk density is 0 * 17g / enA. The appearance is similar to thick malt. shape. These lumps are supplied to an ultrasonic jet mill at a rate of 20 kg / hr to grind to obtain fine dusting material (9). The coloring matter (9) was measured by a Coulter counter (hole 100wm), and its average particle size was 5.81am, and its particle size variation was 17.1%. This fine coloring matter (9) is directly used as a toner for image generation of a still film printer (manufactured by Canon, "NP-5000").结果 如 表 1。 The results are shown in Table 1. (Example 10) A suspension of fine spherical clinker (2) prepared in Example 2 was maintained at 7510, and an aqueous slurry-like modifier (containing 35% of the main component, Tung Hun) was added in advance. Chemical Company, trade name "Bontron S-34") 13 parts and sex micro delta evening powder RQ72 (made by Japan Microsand Corporation) 10 parts scattered in methanol-37-{Please read the precautions on the back before filling this page } This paper is used in size, size, size, size, size, size, size and size (CNS) Grade 4 (210x297 g *)

XbI 經濟部中央櫺準局员工消费合作社印製 五v發明説明（36) 100部之分散掖82·5部，在95°C加熱 1小時製得溶合粒子 塊狀物，用減壓乾燥器在50T：乾燥8小時，得表面局部溶 合結合之粒子1,110部，其容積密度0.26g/cm3,外觀類似 濃麥芽驟粘住粟子狀。此塊狀物以13故/hr速度供給於超 音波噴射粉碎機粉碎製得該徽細著色物（10)。 該微細箸色物（10)經Coulter計數器（孔100 w m)測定，其平均粒徑為6.35am,粒徑變異偽數19.0 \ %。此徹細著色物（10)直接用於靜電影印機（理光公司 製，「Type 4060」）之影像産生用電子照相調色劑。結 果如表1。 (實施例11) 依實施例3製得微細球狀箸色物之懸浮液（3),將此 懸浮液（3)保持於75T,加預先以主成分含置35%之水性 漿狀調整劑（東洋化學公司製，商品名「Bontron S-34 」） 41部及0水指數(39. 5之徼砂10部分散於甲醇100部 之分散液110部，在95 加熱30分得膝合粒子塊狀物， 過濾分離此塊狀物，周減壓乾燥器在50 °C乾燥8小時， 得粒子局部表面馆合結合之塊狀物1,700部，其容積密度 0.202/003.外觀類似濃麥芽膠粘住粟子狀。此20kg/hr 速度供此塊狀物於超音波噴射粉碎機粉碎得微細著色物（ 11)。 侬Coulter計數器（孔100wm)測定結果，此微細 箸色樹（11)之平均粒徑為5* 24 w m ,粒徑變異偽數19· 8% 。此撤細著色物（11)直接用於靜電影印機（佳能公司製 _36 - (請先«'讀背面之注意事項再填寫本頁) 装- 訂 線- 本紙a尺度遴用中a a家揉率(CHS)肀4規格(210x297公龙) £ 035S4 Λ6 B6 經濟部中央搮準局员工消費合作社印製 五、發明説明（37) ,「NP-5000」）之影像産生用電子照相調色劑。結果如 表1。 (實施例12) 侬實施例4製徹細球狀箸色物之懸浮液（4),對此懸 浮液（4)加塗有氯化鍊之氧化錫（三菱金屬製，代號「T-1」 )20部在90^0加熱 2小時製得悠合粒子塊狀物。過 濾分離塊狀物用熱風乾燥機在50t：乾燥10小時，得局部粒 子表面溶合之塊狀物1, 500部，其容積密度為0. 30g/cm3, 外觀類似濃稠麥芽駿粘粟子狀。此18kg/hr 速度供給此 塊狀物於超音波噴射粉碎機粉碎得微細箸色物（12)。 依Coulter計數器（孔100wm)測定此微細箸色物 (12)結果，其平均粒徑6*20um,粒徑變異偽數20.090。 該微細箸色物（12) 直接用於靜電影印機（理光公司製， 「Type 4060」）之影像産生用電子照相調色劑。結果如 表：L 〇 (實施例13) 侬實施例5製得微細球狀著色物懸浮液（5).對此懸 浮液加預先以甲醇100部分散由處理二氣化欽（日本微石夕 公司製，商品名「P25」）而製的水指數15之微細水不 溶性粒子10部之分散液100部及戊院100部，在85 °C加熱 三小時製得熔合粒子塊狀物。過濾分離塊狀物，用減壓草乞 燥機在50X：乾燥八小時，製得各粒子表面部分赌合結合， 容積密度0.34g/ci^,外觀類似濃稠麥芽膠粘住粟子狀之 塊狀物1,500部，將此塊狀物以13kg/hr速度供备於超 -39- 本紙張尺度边用中团8家揉準(CNS) T 4規格(210x297公*) {請先W請背面之注意事項再填窝本頁) 装&lt; 線&lt; 旒濟部中央搮準局Λ工消费合作社印敢 五v發明説明（3S) 音波噴射粉碎機粉碎得微細箸色物（13)。 經Coulter計數器（孔100um)測定結果，該箸色物 (13)之平均粒徑為5·73wnu粒徑變異像數20.5%。該微 細著色物（13)用於靜電影印機（理光公司製，「Type 4060」）之影像産生用電子照相調色劑。結果如表1。 (實施例14) 侬實施例製得微細球狀著色物懸浮液（6)。對此加 由甲醇150部，氣化鉻（日本觸媒化學製，代號「NS-3y 」）15部及粉狀磁性材料（鈦工業公司製，商品名「 Mapico BL-400」）分散製得之分散掖18赔|3,在95X：加 熱1小時，得熔合粒子塊狀物。過濾分離此塊狀物，甩減 壓乾燥機在50TC乾燥8小時，製得粒子表面熔合，容積密 度0· 19g/cn?,外觀類似濃稠麥芽駿粘住粟子狀之塊狀物 1, 500部。將此塊狀以19. 5kg/hr之速度供給於超音波噴射 粉碎機粉碎製得微細著色物（14)。 經Coulter計數器（孔100urn)測定結果，以徽細 箸色物（14)之平均粒徑為6. 21 w m ,粒徑變異偽數21 · 5% 。該微細著色物（14)用於靜電影印機（理光公司製· 「 Type 4060」）之影像産生用電子照相調色劑（14)。結 果如表1 〇 (實施例15) 侬實施例7製得微細球狀箸色物懸浮液（7)。對此懸 浮液，在60¾加戊院200部及預先由甲醇285部，2^水指ί 數64*5之#水性微矽（日本微砂公司製•代號「R80Q」） -40 - (犄先閲请背面之注意事項再填寫本頁&gt; 裝· 線- ·( 条Λ*尺度逍用中a β家楳準(CNS)甲4規格(210x297公龙) Λ 6 Β6 Μ濟部中央搮準屈貝工消费合作社印31 五、發明説明（3¾ 12部，踩水指數50之碎水性微砂（曰本徼砂公司製，代號 「R305」）12部及導電性拔黑（Ketjen 國際公司製，商 品名「KetjenEC」）4·5部分散而成的分散液313部，在 60 C加熱2小時，製得溶合粒子塊狀物。過滤分離此塊 狀物，芾熱風乾燥機在50C乾燥10小時，製得各粒子表面 溶合結合，容積密度0*21g/coA外觀類似濃稠麥芽職粘粟 子狀的塊狀物1,500部。以lSks/hr速度供給此塊狀物於 超音波噴射粉碎機粉碎製得微細著色物（15)。 經 Coulter計數器（孔100 wm)測定結果，以徽 細著色物（15)之平均粒徑為5· 65 μ m ,粒徑變異偽數20. 7 %。此微細著色物（15)直接用於靜電影印機（理光公司 製，「Type 4060」）之影像産生甩電子照相調色劑（ 15)。結果如表1。 (實施例16) 依實施例1之步驟，但不用T.K. Homomixer處理聚合 用箪量體組成物，而以1500rpm混合機（江原製所製，商 品名「Ebara 1 der MDN-3030」）處理五次製得均句懸 浮液，然後加熱於防1C 5小時，再在75C加熱2小時，製 得平均粒徑5. 82 w m ,粒徑變異偽收20. 5%之微細球狀著 色物懸浮液（1’）。此此懸浮液與含主成分5%之氮化錦水 溶液60部混合使徹細球狀箸力物凝集。用離心機分離此凝 集物，在90T：及相對溫度98%下處理10分得悠合粒子塊。 此塊狀物在50^0乾燥則得部份粒子表面熔合結合，容積密 度 0.4g/cm3，外觀類似濃稠麥芽膠粘住粟子狀之塊狀物 -41 - 本紙张又度边用中國Η家《準(CNS)甲4規格(210x297公龙)XbI Ministry of Economic Affairs Central Bureau of Employee's Employee Consumer Cooperative printed the five v invention description (36) 82 disperse parts of 100 parts, heated at 95 ° C for 1 hour to produce fused particle lumps, using a reduced pressure dryer After drying at 50T for 8 hours, there are 1,110 particles that are partially fused and bonded on the surface, with a bulk density of 0.26g / cm3, and the appearance is similar to that of thick malt that suddenly sticks to the millet shape. This mass was supplied to an ultrasonic jet mill at a rate of 13 hr / hr to pulverize to obtain the fine colored substance (10). The fine dust color (10) was measured by a Coulter counter (hole 100 w m), and its average particle size was 6.35am, and the particle size variation pseudo number was 19.0%. This thorough coloring matter (10) is directly used in electrophotographic toners for image production of still film printers (manufactured by Ricoh Corporation, "Type 4060"). The results are shown in Table 1. (Example 11) A suspension (3) of fine spherical clinker was prepared according to Example 3, the suspension (3) was kept at 75T, and an aqueous slurry-like regulator containing 35% of the main component in advance was added (Made by Toyo Chemical Co., Ltd. under the trade name "Bontron S-34") 41 parts and 0 water index (39.5 of 10 parts of Miyasha dispersed in 100 parts of methanol in 110 parts of the dispersion liquid, heated at 95 for 30 minutes to get the kneaded particles Lump, filter and separate the lump, and dry it at 50 ° C for 8 hours with a reduced-pressure dryer to obtain 1,700 pieces of lump combined with the partial surface of the particle, and the bulk density is 0.202 / 003. The appearance is similar to thick malt It sticks to the shape of a millet. This 20kg / hr speed is used to crush this mass in a supersonic jet crusher to obtain a fine coloring matter (11). The measurement result of Nong Coulter counter (hole 100wm), the fine dust color tree (11) The average particle size is 5 * 24 wm, and the particle size variation pseudo-number is 19.8%. This fine color removal material (11) is directly used in the static film printer (made by Canon Inc. _36-(please read the notes on the back first «' (Fill in this page again) 装-线 线-This paper is used in a scale selection of aa home rubbing rate (CHS) 4 specifications (210x297 male dragon) £ 035S4 Λ6 B6 in the Ministry of Economic Affairs Printed by the staff consumer cooperative of the Prefectural Bureau 5. Description of the invention (37), "NP-5000") Electrophotographic toner for image generation. The results are shown in Table 1. (Example 12) Example 4 of Nong made fine balls The suspension (4) of the colored dusty substance is added to this suspension (4) by tin oxide coated with a chlorinated chain (Mitsubishi Metal, codename "T-1") 20 parts are heated at 90 ^ 0 for 2 hours The particles are lumped. Filter and separate the lumps with a hot air dryer at 50t: dry for 10 hours to obtain 1,500 lumps with partial particle surface fusion, with a bulk density of 0.30g / cm3, similar appearance Thick malt sticky millet shape. This 18kg / hr speed is supplied to the lump to be crushed by an ultrasonic jet mill to obtain a fine dust color (12). The fine dust color (12) is measured according to a Coulter counter (hole 100wm) ) As a result, the average particle size is 6 * 20um, and the particle size variation pseudo-number is 20.090. The fine dust color (12) is directly used for electrophotographic toning for image generation of static film printers (manufactured by Ricoh, "Type 4060") The results are shown in the table: L 〇 (Example 13) Nong Example 5 prepared a fine spherical coloring matter suspension (5). This suspension Add 100 parts of methanol to disperse 100 parts of fine water-insoluble particles with a water index of 15 and 100 parts of the Pentium by the treatment of two gasification companies (manufactured by Japan Shishixi Company, trade name "P25") , Heated at 85 ° C for three hours to obtain fused particle lumps. Filter and separate the lumps, and use a reduced-pressure grass dryer to dry at 50X: eight hours to obtain a partial combination of the surface of each particle, bulk density 0.34g / ci ^, the appearance is similar to thick malt gum sticking to 1,500 pieces of millet-shaped masses, this mass is supplied at a speed of 13kg / hr in Chao-39 (CNS) T 4 specification (210x297 g *) (please fill in this page before filling in the precautions on the back of the page) 3S) Sonic jet pulverizer pulverizes fine dust color (13). According to the measurement result of Coulter counter (hole 100um), the average particle size of the color material (13) is 5.73wnu particle size variation image number 20.5%. The fine coloring matter (13) is used in electrophotographic toners for image production of static film printers (manufactured by Ricoh Corporation, "Type 4060").结果 如 表 1。 The results are shown in Table 1. (Example 14) The Nong example prepared a fine spherical coloring matter suspension (6). For this, 150 parts of methanol, 15 parts of chromium vapor (manufactured by Japan Catalyst Chemical Co., Ltd., codenamed "NS-3y") and powdered magnetic materials (manufactured by Titanium Industry Corporation, trade name "Mapico BL-400") were dispersed. The dispersion of 18 compensation | 3, at 95X: heating for 1 hour, to get lumps of fused particles. Separate the lump by filtration and dry it at 50TC for 8 hours with a decompression dryer. The surface of the particles is fused with a bulk density of 0 · 19g / cn ?. The appearance is similar to thick malt sticking to the millet-shaped lump 1. 500. This mass was supplied to a supersonic jet mill at a speed of 19.5 kg / hr to obtain a fine colored substance (14). The Coulter counter (hole 100urn) measured the result, and the average particle size of the fine dust color (14) was 6.21 w m, and the particle size variation pseudo-number was 21.5%. The fine coloring matter (14) is used in an electrophotographic toner (14) for image production of a static film printer (manufactured by Ricoh Corporation "Type 4060"). The results are shown in Table 10 (Example 15). In Example 7, a fine spherical suspension (7) was prepared. For this suspension, add 200 units of Pentium in 60¾ and 285 units of methanol in advance, 2 # water index number 64 * 5 # water-based microsilica (manufactured by Japan Microsand Corporation • codename "R80Q") -40-(焄Please read the precautions on the back first and then fill in this page.> Installation · Line-· (Article Λ * Standard for use a β Jiayu standard (CNS) A 4 specifications (210x297 male dragon) Λ 6 Β6 Μjibu central 殮Printed by the quasi-Quebec industrial consumer cooperative 31 V. Description of the invention (3 ¾ 12 parts, crushed water-based micro-sand with a treading index of 50 (manufactured by Yonabushi Sand Co., codename "R305") 12 parts and conductive black (manufactured by Ketjen International Corporation) , Trade name "KetjenEC") 313 parts of the dispersion liquid divided into 4 and 5 parts are heated at 60 C for 2 hours to prepare a lumped particle mass. The mass is separated by filtration and dried with a hot air dryer at 50C After 10 hours, the surface of each particle was fused and combined, and the bulk density was 0 * 21g / coA. The appearance was similar to 1,500 pieces of thick malt-like sticky millet-shaped pieces. This piece was supplied to ultrasonic jet at a speed of 1Sks / hr. The fine coloring matter (15) is obtained by pulverizing the crusher. The result is measured by a Coulter counter (hole 100 wm), which is equal to the level of the fine coloring matter (15) The average particle size is 5.65 μm, and the particle size variation pseudo-number is 20.7%. This fine coloring matter (15) is directly used in the image generation of static film printer (manufactured by Ricoh, "Type 4060"). Toner (15). The results are shown in Table 1. (Example 16) According to the procedure of Example 1, but not using the TK Homomixer to process the polymer composition for polymerization, a 1500rpm mixer (manufactured by Gangwon, trade name " Ebara 1 der MDN-3030 ") treated five times to prepare a homojunction suspension, then heated at 1C for 5 hours, and then heated at 75C for 2 hours to obtain an average particle size of 5. 82 wm, and a false particle size variation of 20. 5% fine spherical coloring matter suspension (1 '). This suspension is mixed with 60 parts of nitride bromide aqueous solution containing 5% of the main component to agglomerate the fine spherical coagulant. Separate the agglutinate with a centrifuge At 90T: and relative temperature 98% for 10 minutes, you can get a smooth particle block. When this block is dried at 50 ^ 0, part of the particle surface will be fused and combined, the bulk density is 0.4g / cm3, and the appearance is similar to thick malt. Sticking to a millet-shaped lump -41-This paper is edged with the Chinese 掳 揚 Standard (CNS) A 4 specification (210x297 male dragon)

經濟部中央楳準局貞工消费合作社印$L 五、發明説明（斗ο) 1,500部。將此塊狀物粗碎後以llkg/hr速度供給超音波 噴射粉碎機粉碎製得微細箸色物（1S)。 經Coulter計數器測定結果，此微細箸色物（16)之平 均粒徑為5·65^τη，粒徑變異傜數18·8%。該微細箸色物 (1(3)乃直接用於靜電影印機（理光公司製，「Type 4060 」之影像産生用電子照相調色劑（16)。結果如表1。 (實施例17) ' 依實施例2之步驟，但懸浮聚合反應像在65°C進行5 小時然後在75¾ 2小時，製得平均粒徑6.42wm,粒徑變 異偽數21.S%之微細球狀箸色物懸浮液（2’）。次將此懸浮 液（2 ’）在75=0首先與含主成分35%之調整劑，(東徉化學工 業製，商品名「Bontron S-34)之水性駿13部混合，然後 與甲醇1,110部混合使微細球开多箸色物沉澱。過濾分離， 並在801,相對溫度90%下處理20分製得熔合粒子塊。這 塊狀物在50X：乾燥則得，粒子表面部份溶合結合，容積密 度0. 70g/cm3,外觀類似濃稠麥芽膠粘附粟子狀的塊狀物 1,110部。粗碎這塊狀物，以8.0kg/hr速度供給超音波噴 射粉碎機粉碎得微細著色物（17)。 經 Coulter計數器（孔100wm)測定結果，該微 細著色物17)之平均粒徑為6.15wm,粒徑變異偽數23·3 %。此微細箸色物（17)直接用於靜電影印機（理光公司 製，「Type 4060」）之影像産生用電子照相調色劑（17 )。結果如表1。 (實施例18) ' -42-. (請先Μ讀背面之注意事項再墀«本頁} tPrinted by the Ministry of Economic Affairs, Central Habitat Bureau of Zhengong Consumer Cooperative, $ L V. Invention description (fight) 1,500 copies. This mass was coarsely crushed and then supplied to an ultrasonic jet mill at a rate of llkg / hr to pulverize to obtain a fine dust color (1S). According to the measurement result of the Coulter counter, the average particle size of the fine chopstick (16) is 5.65 ^ τη, and the particle size variation is 18.8%. The fine chopsticks (1 (3) are directly used in electrophotographic toners (16) for static image printers (manufactured by Ricoh, "Type 4060"). The results are shown in Table 1. (Example 17) Follow the steps of Example 2, but the suspension polymerization reaction is carried out at 65 ° C for 5 hours and then at 75¾ 2 hours to prepare a fine spherical custard suspended with an average particle size of 6.42wm and a particle size variation pseudo number of 21.S% Liquid (2 '). The suspension (2') is 75 = 0. First, it is prepared with a modifier containing 35% of the main component, (manufactured by Toyo Chemical Industries, trade name "Bontron S-34") 13 parts Mix, then mix with 1,110 parts of methanol to precipitate microspheres. Precipitate by filtration, and process for 20 minutes at 801, 90% relative temperature to obtain a fused particle block. This block is obtained at 50X: dry, Part of the surface of the particles is fused together, the bulk density is 0.70g / cm3, and the appearance is similar to the thick malt gum attached to the millet-shaped mass 1,110. The mass is roughly crushed and supplied with ultrasound at a rate of 8.0kg / hr The fine coloring matter (17) was crushed by the jet mill. The result of the Coulter counter (hole 100wm) measured the level of the fine coloring matter 17). The particle size is 6.15wm, and the particle size variation pseudo number is 23.3%. This fine dust color (17) is directly used in electrophotographic toners for image generation of static film printers (manufactured by Ricoh, "Type 4060") ( 17). The results are shown in Table 1. (Example 18) '-42-. (Please read the precautions on the back first and then «this page} t

T 本泜乐尺度通用中國S家«準(CNS)甲4規格(210x297公¢) Λ 6 Β6 經濟部中央標準扃员工消费合作社印製 五、發明説明（4*1) 依實施例3之步驟，但懸浮聚合反應偽先在&lt;351進行 5小時，然後在75它2小時，製得平均粒徑5·43wm,粒 徑變異偽數22. 5%之微細球狀箸色物懸浮液（3 ’）。此懸浮 液 （3 ’）與75T：與主成分含董35%之水性凝狀調整劑41部 及 5 %氯化館水溶液60部混合，使微細球形著色物粒子 凝集。過濾分離此凝集物•在95 1C,相對溫度100%下 處理 5分使成焰合粒子塊。這塊狀物在50¾乾燥則得粒 子表面部份溶合結合，容積密度0·3δβ/α^外觀類似濃稠 麥芽膠粘住粟子狀的塊狀物1,700部。粗碎此塊狀物，以 13kg/hr之速度供給超音波噴射粉碎機粉碎製得微細著色 物（18)。 經Coulter計數器（孔100wm)測定結果，該微細 箸色物（18)的平均粒徑為5* 22 w m ,粒徑變異像數Ip. 3% 。此撤細著色物（18)用於靜電影印機（佳能公司製，「 ΝΡ 500」）之影像産用電子照相調色劑（1S)。結果如表 1 〇 (實施例19) 侬實施例4之步驟，但懸浮聚合反應改為先在 6510 加熱5小時，然後在75t： 2小時，製得平均粒徑6*30 ,粒徑變異偽數19. 5%之撒細球狀著色物懸浮液（4 ’）。 此懸浮液（4’）與5^；氣化錯水溶液60部混合使微細球狀 著色粒子凝集。過濾分離凝集物，在851C,相對溫度100 %下處理 20分形成熔合粒子塊。此塊狀物在50X：乾燥則 得粒子表面部分熔合結合，容積密度0.31g/ci^,外觀類似 -43- ，· * * ••装· · ·.訂· · · ·線 (請先Μ请背面之注意事項再赛窝本頁) 本紙張尺度逍用中明a家«準(CNS) Τ4規格(210x297公龙)T The standard of the Chinese standard of the Chinese S Home «Zen (CNS) A 4 specifications (210x297 g)) Λ 6 Β6 Printed by the Ministry of Economic Affairs, Central Standards, and Employee Consumer Cooperatives V. Invention description (4 * 1) Follow the steps of Example 3 However, the suspension polymerization reaction was first carried out at &lt; 351 for 5 hours, and then at 75 hours for 2 hours, to prepare a fine spherical clinker suspension with an average particle size of 5.43wm and a particle size variation pseudo number of 22.5% ( 3 '). This suspension (3 ') and 75T: mixed with 41 parts of 35% aqueous coagulation regulator containing the main component and 60 parts of 5% chlorinated water solution to aggregate fine spherical colored particles. Filter to separate this agglomerate. • Treat at 95 1C and 100% relative temperature for 5 minutes to form a mass of flame particles. When this mass was dried at 50¾, the surface of the particles was partially fused and combined, and the bulk density was 0.3 δβ / α ^. The appearance was similar to thick malt gum, which stuck 1,700 pieces of millet-shaped masses. This mass was coarsely crushed and supplied to an ultrasonic jet mill at a rate of 13 kg / hr to obtain a fine coloring matter (18). According to the measurement result of the Coulter counter (hole 100wm), the average particle size of the fine chopsticks (18) is 5 * 22 w m, and the particle size variation image number is Ip. 3%. This fine-removing coloring matter (18) is used in electrophotographic toner (1S) for image production of still film printers (manufactured by Canon Corporation, "NP 500"). The results are shown in Table 10 (Example 19). The procedure of Example 4 was changed, but the suspension polymerization reaction was first heated at 6510 for 5 hours, and then at 75t: 2 hours. The average particle size was 6 * 30, and the particle size variation was pseudo Count 19.5% of the dispersion of fine spherical coloring matter (4 '). This suspension (4 ') was mixed with 5 ^; vaporized water solution in 60 parts to aggregate fine spherical colored particles. The agglomerates were separated by filtration and treated at 851C for 20 minutes at a relative temperature of 100% to form a fused particle mass. This block is at 50X: after drying, the surface of the particles is partially fused and combined, the bulk density is 0.31g / ci ^, and the appearance is similar to -43-, · * * • • installed · · · · · · · · line (please first M Please follow the precautions on the back of this page.) The paper size is easy to use Zhongming a home «quasi (CNS) Τ4 specifications (210x297 male dragon)

66 ΛΒ 經濟部中央搮準局兵工消费合作社印製 五、發明説明（4 2.) 濃稲ί麥芽膠粘住粟子狀的塊狀物1, 500部。粗碎這塊狀物 ，以 15k«/hr速度供給超音波噴射粉碎機粉碎，製得徼 細箸色物（19)。 經 Coulter計數器測試結果，該徽細著色物（19)之 平均粒徑為6* 24 μ m ,粒徑變異偽數20· 8%。此撤細著色 物（19) 直接用於靜電影印機之影像産生兩電子照相調色 劑（19)。結果如表1。 (實施例20) 依實施例5的步驟，但懸浮聚合反應偽在65T：先進行 5小時，然後在75^0 2小時，製得平均粒徑5.92wm,粒 徑變異像數23*.0%之微細著色物懸浮液（5 ’）。此懸浮液與 甲醇混合使撒細球狀箸色粒子沉源。過遽分離，在70T, 相對溫度95%下處理35分形成焰合粒子之塊狀物。此塊狀 物在50π乾燥則得各粒子表面部分馆合結合，容積密度 0.55 g/cm3,外觀類似濃稠麥芽膠粘住粟子狀的塊狀物 1,500部。粗碎這塊狀物，以10.5kg/hr速度供給超音波 噴射粉碎機粉碎，製得微細著色物（20)。 經 Coulter計數器（孔100wm)測試結果，該微 細箸色物之平均粒徑為5.67^ m ,粒徑變異像數21·5%。 該微細著色物（20)直接用於靜電影印機之影像産生甩電 子照相調色劑（20)。結果如表1。 (實施例21) 侬實施例S的步驟，但懸浮聚合反應條件改為先在65 加熱 5小時，然後在75t： 2小時，製得平均粒徑6.02 -44 - (請先Μ请背面之注意事項再填鸾本頁) 装- 線· 本紙張尺度遏用中a a家標準(CNS)甲4規格(210x297公*)66 ΛΒ Printed by the Ordnance Industry Consumer Cooperative of the Central Bureau of Economic Affairs of the Ministry of Economy V. Description of the invention (4 2.) Thick rice malt glued 1,500 pieces of millet-shaped lumps. This block was coarsely crushed and supplied to an ultrasonic jet crusher at a speed of 15k «/ hr to be crushed to obtain a fine dust color (19). According to the test result of Coulter counter, the average particle size of the fine coloring matter (19) is 6 * 24 μm, and the particle size variation pseudo-number is 20.8%. This fine-removing coloring matter (19) is directly used to produce two electrophotographic toners (19) for the image of a static film printer.结果 如 表 1。 The results are shown in Table 1. (Example 20) The procedure of Example 5 was followed, but the suspension polymerization reaction was carried out at 65T: first for 5 hours, then at 75 ^ 0 2 hours, the average particle size was 5.92wm, and the particle size variation image number was 23 * .0 % Fine coloring matter suspension (5 '). This suspension is mixed with methanol to sink fine spherical dust particles to the source. After the separation, it is treated at 70T and a relative temperature of 95% for 35 minutes to form a mass of flame combined particles. This mass is dried at 50π, and the surface of each particle is partially combined. The bulk density is 0.55 g / cm3, and the appearance is similar to the thick malt glue that sticks 1,500 millet-shaped masses. This mass was coarsely crushed and supplied to an ultrasonic jet mill at a rate of 10.5 kg / hr for pulverization to obtain a fine colored substance (20). According to the test result of Coulter counter (hole 100wm), the average particle size of the fine dust color is 5.67 ^ m, and the particle size variation number is 21.5%. The fine coloring matter (20) is directly used in the electrophotographic toner (20) of the static image printer.结果 如 表 1。 The results are shown in Table 1. (Example 21) The procedure of Example S, but the suspension polymerization reaction conditions were changed to first heating at 65 for 5 hours, then at 75t: 2 hours, the average particle size was 6.02 -44-(please pay attention to the back Please fill in this page again.)-Line · This paper is used in the aa home standard (CNS) A 4 specifications (210x297 g *)

五、發明説明（43) 經濟部中央標準局员工消費合作社印製 Λ/m，粒徑變異也數21·2%之撤細箸色物懸浮液（6，）。此 懸浮掖5%氯化齡水溶液180部混合使微細球狀箸色粒子 凝集。過膝分離凝集物，在110ΊΟ,相對溫度100%下處 理3分形成熔合粒子塊。此塊狀物在501C乾燥後得，各粒 子表面溶合結合，容積密度0.51 外觀類似濃掘麥 芽膠粘住粟子狀的塊狀物。粗碎此塊狀物，以 9.5 k/hr 速度供給超音波噴射粉碎機粉碎，製得徼細箸色物（21)。 經Coulter計數器（孔100wm)測試結果，撤細著 色物（21)之平均粒徑為6· 15λ/ m，粒徑變異俗數22·5%。 該徼細箸色物（21)乃用於靜電影印機之影像産生甩電子照 相調色劑（21)。結果如表1。 (實施例22) 侬實施例7之步驟，但懸浮液聚合反應條件改為先在 65Τ：加熱5小時然後在75它2小時，製得平均粒徑5.75w m ,粒徑變異僳數19. 5%之微細球狀箸色物懸浮液（7 ’）。 將此懸浮液與5%氯化錦水溶液180部混合，使微細球狀著 色物粒子凝集。過濾分離此凝集物，在851C相對灘度90% 下處理15分形成熔合粒子塊。在50C乾燥此塊狀物則得， 各粒子部分表面熔合結合，容積密度0.S2g/c^,外觀類 似濃稠麥芽膠粘住粟子狀之塊狀物。粗碎塊狀物，以7kg /hr速度供給超音波噴射粉碎機粉碎，得微細箸色物（22) 〇 經Coulter計數器（孔100wm)測定結果，此微細 箸色物（22)之平均粒徑為5. 65 w m ,粒徑變異像數21.7% -45- (請先閲讀背面之注意事項再填寫本頁) 装. 訂- 線- 本紙張尺度遑用中國家«华(CNS)甲4規格(210x297公¢) Λ 6 Β6 經濟部中央搮準局β工消费合作社印製 五、發明説明（w) 。該撤細著色物（22)直接用於靜電影印機之影像産生用電 子照相調色劑（22)。結果如表1。 (實施例23) 依實施例16之步驟，改以if水性微砂10部分散於甲醇 100部之分散液82. 5部取代 5%氮化錦水溶液，製得焰合 粒子固體物。 然後侬實施例16之步驟製得各粒子部分表面熔合結合 ，容積密度0.39g/cn?,外觀類似濃稠麥芽驟粘住粟子狀 的塊狀物1,50摘5〇粗碎塊狀物，以10kg/hr速度供給超 音波噴射粉碎機粉碎製得撤細著色物（23)。 經 Coulter計數器（孔100um)測定結果，該微 細著色物（23)之平均粒徑為 5·64wm,粒徑變異條數 18*7%。此微細箸色物（23)直接用於靜電影印機之影像 産用電子照相調色劑（23)。結果如表1。 另外，以上述步驟製得凝集微細球狀箸色物，過濾分 離，不經加熱加濕工程，乾燥為密度0.33g/cife塊狀物 。此塊狀物經植型粉碎機粉碎為微細箸色物（23’），其粒 子均成高度球形。此微細著色物（23 ’）測定摩擦電的結果 如表2。 (實施例24) 侬實施例8之步驟製得微細球狀箸色物之懸浮液（1 ’） ，將此懸浮液（1 ’）與5%氯化錦水溶液60部混合使徽細著 色物粒子凝集。如此形成之粒子塊則以連續sp吸引過膝機 分離，沖洗，同時不斷加注於85X：熱水5, 000部中，製得 -45- - ί - (請先Μ请背面之注意事項再填窝本頁}V. Description of the invention (43) Printed by the employee consumer cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs Λ / m, the particle size variation is also 21.2% of the suspension of fine custard (6) This suspension was mixed with 180 parts of a 5% chlorinated aqueous solution to aggregate fine spherical spherical particles. The agglomerates were separated over the knee and treated at 110 ΊΟ for 3 minutes at a relative temperature of 100% to form a mass of fused particles. This mass was obtained after drying at 501C. The surface of each particle was fused and combined, and the bulk density was 0.51. The appearance was similar to thick malt gum sticking to the millet-shaped mass. This mass was coarsely crushed and supplied to an ultrasonic jet crusher at a speed of 9.5 k / hr to be crushed to obtain a fine dusty substance (21). According to the test result of Coulter counter (hole 100wm), the average particle diameter of the fine color (21) is 6.15λ / m, and the particle size variation is 22.5%. The fine pigments (21) are used to produce electrophotographic toners (21) for images from still-film printers.结果 如 表 1。 The results are shown in Table 1. (Example 22) The steps of Example 7 of the embodiment, but the suspension polymerization reaction conditions were changed to 65T: heating for 5 hours and then 75 for 2 hours to obtain an average particle size of 5.75wm, and a particle size variation of 19.5 % Fine spherical globule suspension (7 '). This suspension was mixed with 180 parts of a 5% bromide aqueous solution to aggregate fine spherical colored particles. The agglomerates were separated by filtration, and treated for 15 minutes at 851C relative beach degree of 90% to form a fused particle block. After drying the block at 50C, the surface of each particle is fused and combined, and the bulk density is 0.S2g / c ^, and the appearance is similar to thick malt gum sticking to the millet-shaped block. The coarse crushed lump was fed to an ultrasonic jet mill at a speed of 7kg / hr to obtain a fine dust color (22). The measurement result of the Coulter counter (hole 100wm). The average particle size of the fine dust color (22) 5.65 wm, particle size variation like 21.7% -45- (please read the precautions on the back before filling in this page). Binding-Thread-This paper size is not in Chinese «华 (CNS) A4 specifications (210x297 g) Λ 6 Β6 Printed by the β-Consumer Cooperative of the Central Bureau of Economics of the Ministry of Economy V. Description of Invention (w). The finely-removed coloring matter (22) is directly used for the electrophotographic toner (22) for image production of a still film printer.结果 如 表 1。 The results are shown in Table 1. (Example 23) In accordance with the procedure of Example 16, 10 parts of if aqueous microsand was dispersed in 100 parts of methanol and 82.5 parts of the dispersion was replaced with a 5% bromide aqueous solution to prepare flame-solid particles. Then, the steps of Example 16 were prepared by fusing and bonding the surface of each particle, the bulk density was 0.39g / cn ?, and the appearance was similar to thick malt. , At a speed of 10kg / hr, it was supplied to an ultrasonic jet crusher to obtain a fine colored material (23). The measurement result of the Coulter counter (hole 100um) shows that the average particle diameter of the fine coloring matter (23) is 5.64wm, and the number of particle diameter variations is 18 * 7%. This fine chopstick (23) is directly used as an electrophotographic toner (23) for image production of still film printers.结果 如 表 1。 The results are shown in Table 1. In addition, the agglomerated fine spherical custard was prepared in the above-mentioned steps, filtered and separated, and dried to a mass of 0.33 g / cife without heating and humidification. This lump is crushed into a fine dust color (23 ') by a plant-type crusher, and the particles are all highly spherical. Table 2 shows the results of triboelectric measurement of this fine colored substance (23 '). (Example 24) The process of Example 8 of Example 8 prepared a suspension (1 ') of fine spherical cinder-colored substance, and the suspension (1') was mixed with 60 parts of a 5% chloride aqueous solution to make a fine colored substance Particle agglomeration. The particle block thus formed is attracted to the knee machine by continuous sp to separate and rinse, and is continuously filled in 85X: 5,000 parts of hot water to prepare -45--ί-(please pay attention to the matters on the back first Fill this page}

本紙張尺度道用中國a宋揉準(CNS) Τ4規格(210x297公；¢) 經濟部中央搮準局灵工消费合作社印31 r〇5^d ^' 五、發明説明（45) 各粒子部分表面熔合結合，容積度0.42g/cn^外觀類似 濃稠麥芽膠粘位粟子狀之塊狀物1,500部，粗碎此塊狀物 ，以llkg/hr速度供給此塊狀物於超音波噴射粉碎機粉 碎得微細著色物（24)。 經 Coulter計數器（孔100 wm)測定結果，該箸 色物（24)之平均粒徑為5.60 wm，粒徑變異傷數18.7 %。此微細箸色物直接Μ於靜電影印機之影像産生用電子 照相調色劑（24)。結果如表1。 (實施例25) 依實施例10之步驟製‘得微細球狀著色物之懸浮液（2 ’） ，對此懸浮液（2’），先加有效成分35%之調整劑（東洋化 學工業公司製，商品名「Bontron S-34」）13部，然後加 甲醇1，110部使徹細箸色物粒子沉源。連續吸引過滤此粒 子，在過據機上注加80 ^0熱水4, 000部使其溶合結合粒 子塊。此塊狀物在501C乾燥得各粒子部份表面熔合結合， 容積密度0.70g/cn^,外觀類似濃稠麥芽膠粘住粟子狀之 塊狀物1,110部，粗碎此塊狀物，以8.0kg / hr速度 供給超音波噴射粉碎機粉碎，製得微細著色物（25)。 經Coulter計數器（孔100 am)測定結果，該微 細箸色物 （25)之平均粒徑為6.18 urn,粒徑變異像數 23· 0%。該微細著色物直接用於靜電影印機之影像産生用 電子照相調色劑（25)。結果如表1。 (實施例26) 侬實施例11之步驟製得撤細球狀箸色物之漁浮液（3。 -47- Λ 6 B6 (請先閲讀背面之注意事项再填窝本頁) 裝- 訂- ,ί. 缚▲ 本紙張尺度通用中鼷國家楳準(CNS)甲4規格(210x297公龙) 經濟部中央搮準局员工消费合作社印31 205594 Λ6 _D_6_ 五、發明説明（4§) ，對此懸浮液(3’）與35%調整劑41部及5%氯化鋁水溶液 60部混合使微細著色粒子凝集，以連續式力Π壓過濾此凝集 塊，連鑛力Π注110 °C水3,000音15形成溶合粒子塊，經在 50=乾燥後得各粒子部分表面熔合結合，容積密度0· 35g /c#,外觀類似濃稠麥芽膠粘粟子狀之塊狀物 1,700部 ，此塊狀物粗碎後以13kg/hr速度送進超音波噴射粉碎 機粉碎得微細箸色物（26&gt;。 經 Coulter計數器（孔100wm)測試結果，該徽 細箸色物（26)之平均粒徑為5. 24 w m，粒徑變異偽數19· 0% 。此微細箸色物（26)直接用於靜電影印機（佳能公司製， 「NP-5000」）之影像産生用電子照相調色劑。結果如表 1 〇 (實施例27) 依實施例12之步驟製得徽細球狀箸色物之懸浮液（4 ’） ，混合590氛化錦水溶液60部使微細球跋箸色物凝集。用 離心機分離此凝集物，在留在離心機中狀態下注加851C的 水4, 500部开多成之溶合粒子塊，此塊狀物在50C乾燥，得 各粒子部分表面馆合結合，容積密度0*33g/c^,外觀類 似濃稠麥芽膠粘住粟子狀之塊狀物1,500部，粗碎此塊狀 物，以速；送給超音波噴射粉碎機粉碎製得微 細著色樹（27)。 經Coulter計數器（孔100 am)測試結果，此微 細著色物（27)之平均粒徑為 6.23 wm,粒徑變異係數 20. 5%。將此微細著色物（27)接用於靜電影印機之影像産 生用電子照相調色劑（27)。結果如表1。 -4S - f紙張尺度遑用中fl β家揉準(CHS)甲4規格(210x297公*) ' (請先閲讀背面之注意事項再填窝本頁) 装. 線&lt; Λ 6 13 6 經濟部中央標準局貝工消費合作杜印製 五、發明説明（么7) 4 (實方缶例28) 敗實施例is之步驟製得撤細球狀箸色物之懸浮液（5。 ，此懸浮液與甲醇1,500部混合使徽細球狀箸色物沉雜， 以離心機分離此沉澱，注加75”水S，000部形成熔合粒子 塊，在50°C乾燥後得，各粒子表面部分熔合結合，容積密 度0.55g/cn^外觀類似濃循麥穿膠粘注粟子狀之塊狀物 1,500部，粗碎後供給超音波噴射粉碎機粉碎，製得撤細 箸色物（28) ,:, 以 Coulter計數器（孔100 um)測試結果，此徽 細箸色樹（28〉之平均粒徑為5. 65 a m ,粒徑變異偽數21 · 6 %。將此徽細著色樹（28)直接用於靜電影印機之影像産生 兩電子照相調色劑（28) c，結果如表1。 ί實施例29) 欲實施例14之步驟製得微細球狀箸色物之愍浮液（6 ’） ，將此懸浮液（6’）與 5%氯化Μ水溶液130部混合凝集。 以連鑲式壓遽機滅取凝集物，連繽注加 115”之水4, 000 部形成溶合粒子塊，在50°C乾燥後得各粒子表面結合燈合 ，容積密度0*53g/cr^外觀類拟濃循麥穿膠結粟子狀之 塊狀物1，500部，粗碎之，以S*5kg/hr速度(共給超音波 喷射粉碎機粉碎，製得微細箸色物（29)。 以Coulter計數器（孔100am)测試結果，此微細 箸色物（29)之平均粒徑為6.12“ m ,粒徑變異偽數22·3% 。此微細箸色物（29)直接用於靜電影印機之影像産生兩： 子照相識色劑（29)。結果如表1。 * -49 - (請先閲讀背面之注意事項再璜寫本頁) 装&lt; 訂- 線&lt; 本紙張尺度遑用中团田家«準(CNS)肀4規格(210x297公¢) 66 ΛΒ 經濟部中央標準局员工消费合作社印31 五、發明説明（年&amp;) (¾施例S0) 依實施例15之步驟製得微細球狀替色物懸浮寂（7。， 與甲醇1，500部及工業级乙_混合，使箸色換沉澱，以連 續式吸引過滅機分離此沉雜，以90T：熱水2,500部沖洗加 熱形或溶合粒子塊，在50t〕乾燥得各粒子表面部分熔合結 合，容積密度8· 62g/cr^外觀類似濃循麥穿驟钻粟子狀 之塊狀樹1,500部，粗碎之，以7kg/hr速度供給超音波 噴射粉碎機粉辟，製得徼細箸色物（30)。 以Coulter計數器（孔100am)測試結果，該徽細 箸色物（30)之平均粒徑為5· 61 wm，粒徑變異偽數21· 5 %。該微細著色物（30)直接兩於靜電影印機之影ί象産生 兩電子照相調色劑（S0)。結果如表1。 (實施例S1) 砍實施例24之步驟凝集微細球狀箸色物製得熔合粒子 塊，並過濾分離此熔合粒子塊，但偽以預先將殊水姓微砂 10部及導電性炭黑3部分散於甲醇130部之分散液143部 取代5 96氯化辑水；容者。 然後依實施例24之步驟製得各粒子部分表面溶合結合 ，容積密度0·302/α^,外觀類似濃擺麥穿膠'結住粟子狀 之塊狀樹1,500部。粗碎之，以12kg/hr速度供給超音波 噴射粉碎機粉辟，製得徹細著色物（S1)。 以 Coulter計數器（孔100am)測定結栗，微細 箸色物（S1)之平均粒徑為5. 43 ^ m，粒徑變異ί条數17.8¾ 。該微細箸色物（31)直接用於靜電影印機之影像産用電 -50- (請先閲請背面之注意事項再嶙窝本頁) 装&lt; 訂· 線· 本紙張尺度ϋ用中a a茱椹導(CNS)甲4規格(210χ297公龙) 經濟部中央標举局员工消费合作社印製 五、發明説明（的） 子照相調色劑（S1)。結果如表1 另依上述步驟，凝集竝分離熔合粒子塊，不經加熱及 加濕處理，乾燥後得體積為密度0*26g/c^之塊狀物。以 植磨機粉碎機粉碎此塊狀物.製得徼細著色物（31’），其 球形極為良好，該徽細箸色物.（S1')測定摩擦帶電的結 果如表2。 (比較例1 ) 將在實施例4製得之微細球狀箸色物之懸浮液（4) 10，480部保持於75=〇,加氛化錦 5部，加歷下加熱於 1501 30分製得馆合粒子塊，過據，減壓乾燥（50°C，S 小時），粗碎之，以4kg/&quot;hr速度供給·同一超音波噴射粉 碎機粉碎，製得比較用徼細箸色物（a) 1,500部。 該微細箸色物（a)測試其徽粒微特柱，直接用於靜電 影印機（理光公司製，「Type 4060」之影像産生用電子 照相調色劑（a)以資比較。結果如表1。 (比較例2) 依實施例4之步驟製得之微細球狀著色樹，但因懸浮 聚合反應像在S5X：進行4小時，因此變換率為36%,當此 微細球狀箸色物再加熱於2小時後，粒子則形成一大 凝聚塊，不易再進行往後處理。 (比較例3) 使兩加壓煉合機，將苯乙嫌—丙締酸樹脂（三洋化成 公司製，代號「78-1000「」）2,228部，炭黑187部（三 變化學工業公司製，化號「MA-100R」187部，及調整劑（ -51 - Λ 6 13 6 ····*······**···( ··♦·*·· 4^&gt;»···-'ι7·-····· ^^ ··· ·( (請先Μ請背面之注意事項再填窝本頁) 本紙5fc尺度ϋ用中团國家標準(CNS)肀4規格(210x297公¢) Λ6 D6 經濟部中央搮準局员工消资合作社印31 五、發明説明（50) 保土谷化學公司製，商品名「Aizen Spilon Blacr TRH」 )在150^0煉合S0分，然後冷卻，得調色劑塊。將此調色 劑塊打碎成0· 1至2mm小塊，然後以實施例1所角超音波噴 射粉碎機粉碎為微粉，以送風分綴機（日本氣動工業公司 製，化號「DS-2型」）分级製得比較周徽細箸色物 （b) 1,500部。 測試其徽粒性狀後將此比較用擻細著色物（b)直接用 於靜電影印機（理光公司製，4060型）之影像産生闱電子 照相調色劑⑹，結果如表1。 (比較例4) · 侬實施例19之步驟製得微細球狀著色物之熔合塊，在 力Π歷下以1401，相對濕度100%處理，在50°C乾燥後得 塊狀物1,500部。粗碎之，以2kg/hr速度供給實施例4 戸斤用粉碎機粉碎，製得比較炤徽細箸色樹（〇 ,測試其徽 粒性狀後直接炤於靜電影印機之影像産生兩電子照相調色 劑（e)。結果如表1。 (比較例5) 依實施例19之步驟製得微細球狀替色物之過濾物，在 851，相對濕度60%下處理20分後形成的塊狀物的組成粒 實質上並沒有溶合。該塊狀物在 50 °C乾燥後得塊狀物 1,500部。粗碎之，以 20kg/hr速度供給實施例4所闬 粉碎機粉碎，製得比較用徽細著色軟I (〇0,經電子掃猫 微寫器檢査結果，該比較周微細著色物（d)之Q0%以上係 球形，這顯示加熱，加濕處理幾乎不産生效果。.比較兩徼 {請先閲讀背面之注意事項再琪窝本頁) 本紙法尺度通用中a國家樣準(CNS)甲4規格(210x297公4) A 6 13 6 經濟部中央楳準局貝工消费合作杜印製 五、發明説明（Ξ1) 細著色體⑺）測試其德I粒性狀，並用於靜電影印機之影像 産生用電子照相調色劑（d)。結果如表1。 (比較例6) 依實施例27之步驟製得徽細球形著色樹之含水凝集物 。以連續壓濾法去除掖體，沖洗濾渣，連續注加135°C熱 水3, 000部形成溶合粒子塊，在5KC乾燥得塊狀物 1,500 部。粗碎之，以 2kg/hr速度供給實施例27之粉碎機粉 碎，製得比較用微細箸色物（e)。 測試此比較用徼細著色物（e)之微粒性質，直接芾於 靜電影印機之影像産生用電·子照相調色劑（e)，結果如表 1 〇 (比較例7) 依實施例27之步驟製得徽細球形箸色物之含水凝集物 。以離心法分離水分，連鑲以45°C熱水3,000部加注於離 心機上之濾澄得實質上沒有溶合的粒子，這在50_3C乾燥後 得塊狀ί勿 1，500部。粗碑此塊狀拽，以20kg/hr之速 度供給實施例 27所闱之粉碎機粉碎，製得比較周微細著 色物 （f)。以電子掃瞄顯寫機測驗此比較用微細著色ΐ匆 的結果顯示，90%以上偽球狀，這顔示加熱，加濃處理幾 乎不産生效果。 該比較周微細箸色掏（f)檢驗其微粒性狀，並直接周 於靜電影印機之影像産生用電子照相調色劑（〇，結果如 表1 〇 (比較例8 ) -53 - {«先閲請背面之注意事項再場窝本頁} 裝- 線- 本紙51尺度边用中8困家楳华(CNS)甲4規格(210x297公龙) 經濟部中央橾準局员工消费合作社印製 L0咖4 Λ6 ___B6__ 五、發明説明（52) 依實施例1δ之步驟製得懸浮液（1。，混合5%氮化培 水溶液100部使徽細球狀替色樹凝集,:，過遽分離乾燥後， 不做力Π熱、加篇處理，得容積密度0.23g/cn?之塊狀物， 再以植磨機粉碎製得比較用微細箸色物（S),測驗磨擦帶 電的結果如表2。 表1·(續前） (備註1)粉碑量：供給於超音波噴射粉碎機（日本氣動工業 公司製，代號” [DS2型」）之量為粉碎量。 (備註2)粒徑：以Coui ter計數器測試（Cou丨ter電子公司 司製，代號Γ·ΤΑ-ΙΙ」）。 ， 粒徑變異偽數：以Coulter計數器測試（同上） ‘磨擦帶電量：以鐵擔體（同和鐵粉公司，代號「DSP -128)並用吹粉電苘S式驗器（東芝化學公司製， 代號 r?4odel TB-200」） 流動性：調色劑之流動性偽茁目視評估分四级。 〇:各調色劑粒子完金獨立且流動極好。 〇 :稍有凝集，各調色粒之流動性普通。 △:有凝集，各調色粒流動性差。 X :嚴重凝集，各調色粒流動極不良。 (備註3):影像産生之評估：以影印機（理光製40*30型， 或佳能製NP5000型）影印複製No.l試圖，評估。 模猢：由供試調色劑有無模糊來區別.:、 細線再現性：以複製鼷No· 1影印圖檢査亦跡。 清晰性：以複製匾Ν〇· 1影印，由影印_評估澝晰程度。 一 54 — ^_紙张尺度A用中國S家棋準(CNS)T4規格(210x25)7公;*) f請先閲讀背面之注意事項再填茸本頁} 装· 訂· ,05½ ί» Λ 6 13 6 五、發明説明（53j 躪!§?S6 511,2 Flill iissllw! (6) (7) .§!!!FlisThis paper is based on China ’s Song Song Standard (CNS) Τ4 specifications (210x297 g; ¢) 31 R〇5 ^ d ^ 'printed by the Lingong Consumer Cooperative of the Central Bureau of Economic Affairs of the Ministry of Economy V. Description of the invention (45) Each particle part The surface is fused and combined, and the volume is 0.42g / cn ^. The appearance is similar to the thick malt adhesive position. 1,500 pieces of millet-shaped pieces. The pieces are roughly crushed and supplied to the ultrasonic jet at a speed of llkg / hr. The pulverizer pulverizes to obtain fine coloring matter (24). According to the measurement result of the Coulter counter (hole 100 wm), the average particle size of the color material (24) is 5.60 wm, and the number of particle size variations is 18.7%. This fine dust color material is directly used in the electrophotographic toner (24) for image generation of a still film printer.结果 如 表 1。 The results are shown in Table 1. (Example 25) According to the procedure of Example 10, a suspension of fine spherical coloring matter (2 ') was prepared. To this suspension (2'), a modifier of 35% of the active ingredient was first added (Toyo Chemical Industry Co., Ltd.) System, trade name "Bontron S-34"), 13 parts, and then add 1,110 parts of methanol to sink the fine dust particles. Continuously attract and filter the particles, and add 4,000 parts of 80 ^ 0 hot water to the filter machine to fuse and bind the particles. The block was dried at 501C, and the surface of each particle was fused and combined, with a bulk density of 0.70g / cn ^. The appearance was similar to thick malt gum sticking to 1,110 parts of the millet-shaped block. 8.0 kg / hr speed is supplied to the ultrasonic jet mill to pulverize to obtain fine coloring matter (25). According to the measurement result of Coulter counter (hole 100 am), the average particle size of the fine chopsticks (25) is 6.18 urn, and the particle size variation image number is 23.0%. The fine coloring matter is directly used in electrophotographic toner (25) for image production of static film printers.结果 如 表 1。 The results are shown in Table 1. (Embodiment 26) The steps of Example 11 of Nong made a fishing float with fine ball-shaped chopsticks removed (3. -47- Λ 6 B6 (please read the precautions on the back before filling the nest page). -, ί. Binding ▲ This paper standard is common to China National Standards (CNS) A 4 specifications (210x297 gongs). The Ministry of Economic Affairs, Central Bureau of Preservation and Employee's Consumer Cooperative Printed 31 205594 Λ6 _D_6_ V. Description of Invention (4§), yes This suspension (3 ') is mixed with 41 parts of 35% modifier and 60 parts of 5% aluminum chloride aqueous solution to agglomerate the fine colored particles, and the agglomerate is filtered by continuous force pressure, and the mineral force is injected with 110 ° C water 3,000 tone 15 forms a fused particle block. After 50 = drying, the surface of each particle part is fused and bonded. The bulk density is 0. 35g / c #. The appearance is similar to thick malt glued millet-shaped lump. The material was coarsely crushed and sent to an ultrasonic jet crusher at a speed of 13kg / hr to be crushed to obtain a fine dust color (26>. After the Coulter counter (hole 100wm) test result, the average particle size of the emblem fine dust color (26) It is 5. 24 wm, and the particle size variation pseudo number is 19 · 0%. This fine chopstick (26) is directly used in a static film printer (manufactured by Canon, "NP-5000") electrophotographic toner for image generation. The results are shown in Table 10. (Example 27) A suspension (4 ') of fine spherical globule color was prepared according to the procedure of Example 12 and mixed 590 Aqueous bromide aqueous solution 60 parts agglomerate the fine ball dust. Separate the agglomerate with a centrifuge, and inject 851C water while leaving in the centrifuge. The block is dried at 50C, and the surface of each particle is combined and combined, the bulk density is 0 * 33g / c ^, and the appearance is similar to thick malt glue sticking to 1,500 pieces of millet-shaped blocks, and the block is coarsely crushed. At a speed; sent to ultrasonic jet mill to make fine coloring tree (27). After the test result of Coulter counter (hole 100 am), the average particle size of this fine coloring matter (27) is 6.23 wm, the coefficient of variation of particle size 20. 5%. This fine coloring matter (27) is applied to the electrophotographic toner (27) for image production of static film printers. The results are shown in Table 1. -4S-f paper scale used in domestic fl β home kneading Standard (CHS) A4 specifications (210x297 g *) '(please read the precautions on the back before filling the nest page). Install. Thread & Λ 6 13 6 warp 5. Printed by the Ministry of Economy, Central Bureau of Standards, Shellfish Consumer Cooperation V. Description of the invention (Mo 7) 4 (Square Example 28) The procedure of Example is is to obtain a suspension of fine-ball-shaped chopsticks (5., This suspension was mixed with 1,500 parts of methanol to make the fine spherical globule dusty. Separate the precipitate with a centrifuge, and add 75 ”water to S.000 parts to form a fused particle block. After drying at 50 ° C, each particle The surface part is fused and combined, and the bulk density is 0.55g / cn ^. The appearance is similar to thick 1500 wheat. The lumps of millet-shaped blocks are glued and then crushed and supplied to an ultrasonic jet crusher for crushing. ),:, Based on the Coulter counter (hole 100 um) test results, the average particle size of this emblem is 28.65 am, and the particle size variation pseudo-number is 21.6%. The thin colored tree (28) is used directly to produce two electrophotographic toners (28) c for the image of a static film printer. The results are shown in Table 1. Example 29) To obtain a floating liquid (6 ') of fine spherical clinker by the procedure of Example 14, this suspension (6') was mixed with 130 parts of 5% M chloride aqueous solution and aggregated. The condensate is extinguished with a continuous press, and 4,000 pieces of 115 ”of water are added to form a fused particle block. After drying at 50 ° C, the surface of each particle is combined with a lamp, and the bulk density is 0 * 53g / cr ^ Appearance-like pseudo-condensed millet-shaped lump-shaped lump of 1,500 pieces, coarsely crushed, at a speed of S * 5kg / hr (to be crushed by an ultrasonic jet mill to produce fine dusty color (29 ). Based on the Coulter counter (hole 100am) test results, the average particle size of this fine dust color (29) is 6.12 ”m, and the particle size variation pseudo number is 22.3%. This fine dust color (29) is used directly Two images are produced on the static film printer: Subphotographic Recognizer (29). The results are shown in Table 1. * -49-(Please read the precautions on the back before writing this page) Install &lt; Order-Line &lt; This The paper standard is not used. The Zhongtuan Tianjia «quasi (CNS) 4 specifications (210x297 g) 66 ΛΒ Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 31 V. Description of the invention (year &amp;) (¾Example S0) According to the example 15 steps to prepare fine spherical color substitutes suspended (7., mixed with 1,500 methanol and industrial grade B_, make the color change to precipitate, and continuously attract the extinction machine. This complex, with 90T: 2,500 hot water to wash the heated or fused particle block, dried at 50t] to get the surface of each particle fused and joined, the bulk density is 8.62g / cr ^, the appearance is similar to the thick drilled wheat 1,500 pieces of massive trees, coarsely crushed, supplied to the ultrasonic jet crusher at 7kg / hr, to obtain a fine dust color (30). Based on the Coulter counter (hole 100am) test result, the emblem fine dust The average particle size of the color material (30) is 5.61 wm, and the particle size variation pseudo-number is 21.5%. The fine color material (30) is directly applied to the image of the static film printer to produce two electrophotographic toners ( S0). The results are shown in Table 1. (Example S1) Cut the steps of Example 24 to agglomerate fine spherical dust to produce a fused particle block, and filter to separate the fused particle block. 10 parts and 3 parts of conductive carbon black dispersed in the 130 parts of methanol, 143 parts of the dispersion liquid instead of 5 96 chlorinated water; content. Then follow the steps of Example 24 to obtain the surface of each particle part fusion bonding, bulk density 0 · 302 / α ^, the appearance is similar to that of thick wheat squeezing through the rubber ', which has 1,500 lumpy tree blocks. 2kg / hr speed is supplied to the supersonic jet pulverizer to obtain a fine coloring matter (S1). The Coulter counter (hole 100am) is used to measure the chestnut, and the average particle size of the fine dust coloring matter (S1) is 5.43 ^ m, the particle size variation number 17.8¾. The fine dust color (31) is directly used for the image production of static film printers-50- (please read the precautions on the back and then this page) Install &lt; Order · Line · The paper size ϋ used in the aa Zhu Zhu guide (CNS) A 4 specifications (210 × 297 male dragon) Ministry of Economic Affairs Central Examination Bureau staff consumer cooperatives printed five, invention description (of) sub-photographic toner ( S1). The results are shown in Table 1. According to the above steps, the fused particles are aggregated and separated without heating and humidification. After drying, a mass with a density of 0 * 26g / c ^ is obtained. This block was crushed by a plant mill grinder. The fine colored substance (31 ') was obtained, and its spherical shape was extremely good. The emblem was a fine colored substance. (S1') The results of triboelectric charging are shown in Table 2. (Comparative Example 1) 10,480 parts of the suspension of fine spherical custard material prepared in Example 4 (4) were kept at 75 = 〇, 5 parts of chlorinated broth were added, and heated to 1501 for 30 minutes under the additional calendar Obtained the compound particle block, obtained the data, dried under reduced pressure (50 ° C, S hours), coarsely crushed it, supplied at 4kg / &quot; hr speed, crushed by the same ultrasonic jet crusher, and prepared a relatively fine powder Colors (a) 1,500. The fine chopsticks (a) were tested for their micro-grain micro-pillars, which were directly used in static film printers (manufactured by Ricoh Co., Ltd., "Type 4060") electrophotographic toner (a) for image generation. The results are shown in the table. 1. (Comparative Example 2) The fine spherical colored tree prepared according to the procedure of Example 4, but due to the suspension polymerization reaction like in S5X: 4 hours, so the conversion rate is 36%, when this fine spherical dust After reheating for 2 hours, the particles formed a large agglomerate, making it difficult to carry out further processing. (Comparative Example 3) Using two pressure kneaders, styrene-acrylic resin (manufactured by Sanyo Chemical Co., Ltd., Code "78-1000" "2,228 parts, carbon black 187 parts (manufactured by Sankei Industry Co., Ltd., chemical code" MA-100R "187 parts, and regulator (-51-Λ 6 13 6 ···· ** ····· ** ·· ((·· ♦ · * ·· 4 ^ &gt; »··· -'ι7 ·-····· ^^ ···· ((Please first please back Matters needing attention and refill this page) The 5fc scale of this paper is used in the Chinese National Standards (CNS) 4 specifications (210x297 g). Λ6 D6 Printed by the Employee Expenditure Cooperative of the Central Bureau of Economic Affairs of the Ministry of Economics 31 V. Description of Invention (50) Guarantee Tsuchiya Chemical Produced by the company, with the trade name "Aizen Spilon Blacr TRH") S150 points are blended at 150 ^ 0, and then cooled to obtain a toner block. This toner block is broken into small pieces of 0.1 to 2 mm, and then implemented In Example 1, the supersonic jet pulverizer was pulverized into fine powder, and the comparative Zhou Hui fine dust color (b) 1,500 parts was prepared by grading with an air distribution machine (manufactured by Japan Pneumatic Industry Corporation, chemical number "DS-2"). After testing the character of the emblem, use the fine coloring matter (b) directly to produce the electrophotographic toner ⑹ of the image of static film printer (manufactured by Ricoh Co., Ltd. Model 4060). The results are shown in Table 1. (Comparative Example 4) · The fused block of fine spherical coloring material was prepared by the steps of Example 19, treated with 1401 and 100% relative humidity under force, and dried at 50 ° C to obtain 1,500 blocks. , Supplied to Example 4 at a speed of 2kg / hr. Crushed with a grinder to produce a relatively thin color tree (○, after testing the shape of the emblem, the image was directly placed on the image of the static film printer to produce two electrophotographic toners (E). The results are shown in Table 1. (Comparative Example 5) Filtration of fine spherical color substitutes prepared according to the procedure of Example 19 The lumps formed in the lumps formed after treatment for 20 minutes at 851 and relative humidity of 60% did not substantially dissolve. The lumps were dried at 50 ° C to obtain 1,500 lumps. It was supplied to the holm mill in Example 4 at 20kg / hr for grinding, and the comparatively fine colored soft I (〇0, which was checked by the electronic scanning cat micrograph, was compared, and the Q0% of the finely colored substance (d) was compared. The above is spherical, which shows that heating and humidification treatment have little effect. .Compare the two (please read the precautions on the back and then Qiwo page) The standard of this paper is the national standard (CNS) A 4 specifications (210x297 g) A 6 13 6 Central Bureau of Economics, Ministry of Economic Affairs Consumer Cooperation Du Printing V. Description of the Invention (Ξ1) Fine color body ⑺) Test the properties of its particles, and use it for electrophotographic toner (d) for image production of static film printers.结果 如 表 1。 The results are shown in Table 1. (Comparative Example 6) According to the procedure of Example 27, an aqueous agglomerate of a finely colored spherical tree was prepared. The filter body was removed by continuous pressure filtration, the filter residue was rinsed, and 3,000 parts of hot water at 135 ° C were continuously injected to form a fused particle block, which was dried at 5KC to obtain 1,500 blocks. The coarsely crushed powder was supplied to the pulverizer of Example 27 at a rate of 2 kg / hr to obtain a fine dust color (e) for comparison. The particle properties of the fine coloring matter (e) used for this comparison were tested, and the electrophotographic toner (e) used for image generation directly on the static film printer was used. The results are shown in Table 1 (Comparative Example 7). According to Example 27 The steps are to prepare water-like agglomerates of fine spherical cinder-colored objects. Separate the water by centrifugal method, inlay 3,000 parts of 45 ° C hot water on the centrifuge, and filter it to be substantially free of dissolved particles. After drying at 50_3C, there will be lumpy 1,500 parts. The rough monument was dragged in a block shape, and was supplied to the pulverizer of Example 27 at a rate of 20 kg / hr for pulverization to obtain a relatively fine colored substance (f). The results of this comparison using micro-coloring were tested with an electronic scanning display writer. The results showed that more than 90% were pseudo-spherical, which showed that the heating and thickening treatment had almost no effect. The comparison is made with a fine-grained color (f) to check its particle properties, and it is directly used for electrophotographic toners for image generation of static film printers (〇, the results are shown in Table 1 〇 (Comparative Example 8) -53-{«先Please read the precautions on the back page for the next page.} Install-Thread-51 sheets of paper for the size of 8 in the middle of the sleepy family (CNS) A 4 specifications (210x297 male dragons) Printed L0 by the Employee Consumer Cooperative of the Central Ministry of Economic Affairs Coffee 4 Λ6 ___B6__ V. Description of the invention (52) The suspension was prepared according to the procedure of Example 1 δ (1. Mix 100 parts of 5% nitriding aqueous solution to agglomerate the fine ball-shaped color-changing tree.:, Separate and dry After no heat and heat treatment, a block with a bulk density of 0.23g / cn? Was obtained, which was then crushed with a plant mill to obtain a fine duster (S) for comparison. 2. Table 1. · (Continued) (Remark 1) The amount of powder: the amount supplied to the ultrasonic jet mill (manufactured by Japan Pneumatic Industry Co., Ltd., codenamed "DS2 type") is the crushing amount. (Remark 2) Particle size : Test with Couiter counter (manufactured by Couter Electronics Co., codename Γ · ΤΑ-ΙΙ)., Pseudo-number of particle size variation: Coulter Counter test (same as above) 'Frictional charge: using iron support (Tonghe Iron Powder Company, code-named "DSP-128) and using powder-blown electric pyrene S type tester (manufactured by Toshiba Chemical Company, code-named r? 4odel TB-200" ) Fluidity: The toner ’s fluidity is evaluated visually in four grades. ○: Each toner particle is completely independent and has excellent flow. 〇: Slightly agglomerated, the fluidity of each toner particle is normal. △: There is agglomeration, and the flowability of each toner is poor. X: Severe agglomeration, the flow of each toner is extremely poor. (Remark 3): Evaluation of image generation: using a photocopier (40 * 30 manufactured by Ricoh, or NP5000 manufactured by Canon) Photocopying copy No. 1 is tried and evaluated. Moo: It is distinguished by whether the test toner has blur.:, Thin line reproducibility: It is also checked by copying No. 1 photocopy image. Clarity: Copying plaque Ν〇 · 1 Photocopy, from the photocopy _ to assess the degree of clarity. Yi 54 — ^ _Paper size A uses China S home chess standard (CNS) T4 specifications (210x25) 7 g; *) f Please read the notes on the back before filling This page} Binding · Order ·, 05½ ί »Λ 6 13 6 V. Description of the invention (53j 躏! §? S6 511,2 Flill iissllw! (6) (7) .§ !!! Flis

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I I I 筇丨項丨眾丨項 I I I ¾ 經濟部中央標準局员工消费合作杜印31 H~~h iswitl 00^ ^s. My OT· k— yp· 銪 Ιϋ 銪 15®』 砰—¾ ΐ—別— m 5 本紙張尺度边用中a a家谍準（CHS)肀4規格（2〗ClX297公龙） 铕卜I哲丨銪 III 珂j砰丨荈丨p· I I I 項丨頌I眾丨笱 銪 a苕 il riii 裔 ί-ff(30rf;a90%RH) »0 0^ il i § ^〇5〇94 Λ 6 13 6 五、發明説明（57) 表 2 箸色物（23’） 著色物（3Γ) 分劃著色物（g) mnuvmQ% m -25.8 uC/g -21.8 «C/g -22.0 uC/g _i_y0娜襲 -25.6 uC/g -20.9 aC/g -12.4 iiC/g (請先閲讀背面之注意事項再填寫本頁) 装· 訂· 線 經濟部中央搮準局貝工消费合作社印製 —5 9 — 本紙張尺度通用中國困家榣準(CNS)甲4規格(210x297公¢)III 歇 丨 Item 丨 Public 丨 Item III ¾ Employee Consumption Cooperation of the Central Bureau of Standards of the Ministry of Economic Affairs Du Yin 31 H ~~ h iswitl 00 ^ ^ s. — M 5 The size of the paper is used in the middle of the aa home espionage (CHS) 4 specifications (2〗 ClX297 male dragon) Europium I Zheshu Europium III Kej Bang Shu Piao III Item Shun I Zhong Shu Jia苕 il riii 並 ί-ff (30rf; a90% RH) »0 0 ^ il i § ^ 〇5〇94 Λ 6 13 6 V. Description of the invention (57) Table 2 Colors (23 ') Colors ( 3Γ) Division coloring matter (g) mnuvmQ% m -25.8 uC / g -21.8 «C / g -22.0 uC / g _i_y0 娜 袭 -25.6 uC / g -20.9 aC / g -12.4 iiC / g (please read first Note on the back and then fill out this page) Installation · Order · Printed by Beigong Consumer Cooperative of Central Accreditation Bureau of the Ministry of Economic Affairs — 5 9 — This paper standard is common to China's Sleepy Family Standard (CNS) A 4 specifications (210x297 g)

Claims (1)

嫌濟部中*揉準爲员工消#合作社印« 號「著色微粒子 使用該微粒子之電子攝影用 由舍畜室重来&quot;齡隨砍7TT女 六、申請專利範園 1·—種著色撇粒子之製造方法，其特擻為：將聚合用單釐 '體懸浮於懸浮媒體，在箸色劑及/或磁性粉之存在下進 行懸浮聚合，形成平均粒徑3到50 w m之微細球形蠆色 賭，然後以水為力卩熱媒在50°C到130¾範圍加熱此微細 球形箸色藤，由此使著色體粒産生溶合而該塊狀物，然 後藉粉碎該塊狀物製得粒徑實質上與未熔合前之撇細著 色龌粒子之平均粒徑相同者。 2·如申請專利範園第1項之方法，其中，熱處理係隨懸浮 聚合後，以該微細著色體在水溶媒之懸浮狀下進行者。 3·—種箸色微粒子之製造方法，其特擻為：將聚合用單童 體懸浮於懸浮媒體，在著色劑及/或磁性粉之存在下進 行懸浮聚合，製得平均粒徑3到50 w m之微細球形著色 體懸浮液，然後將此懸浮液力Π熱至501C到98¾使其聚合 ，同時使該粒子焰合成塊狀物，再將此塊狀物粉碎製得 實質上與未熔合前之微細箸色髏粒子之平均粒徑相同者 Ο 4·如申請專利範圔第3項之方法，其中，微細塊狀箸色體 在懸浮聚合液中之變換為粒子熔合者為9090或以上者。 5.—種箸色微粒子之製造方法，其特徽為：在箸色劑及/ 或磁性粉之存在下，將聚合用單量體懸浮於懸浮媒體進 行懸浮聚合，製得平均粒徑3到50 λζ m之粒子佔9090或 以上之微細箸色物，而對此混合物⑴加微細不溶於水 之粒子，及（2)在50°C至98°C範圍加熱處理，進行聚合 ，同時使該微細球狀著色體焰合成焰合粒子塊，然後粉 -1 - (請先閱讀背面之注意事項再填寫本I&gt; 丨裝· 訂. •線. 本·纸張尺度適《中··家嫌準（CNS)甲4规格（210 X 297公釐） β濟部申夬襻準局Λ工消费合作杜印W β7 C7 D7 ___ 六、申請專利範团 碎此塊狀物製得其平均粒徑實質上與未焰合前之微細球 狀色著色體之平均粒徑相同者。 6·如申請專利範圍第5項之方法，其中之水不溶性微細粒 子之水指數為5以上者: 7·如申請專利範圍第5項之方法 &lt; 其中之水不溶性微細粒 子為微細導霣性粒子,。 8·如申請專利範園第2項之方法，其中，在焰合處理前偽 加入對微細球狀箸色物樹脂之溶解性不佳之有機溶劑者 Ο 9·如申請專利範園第5項之方法，其中，在粒子焰合處理 前傲力Π入對微細球狀著色物樹脂之溶解性不佳之有機溶 劑者。 10·如申請專利範圍第1項之方法，其中，該熱處理偽對由 懸浮媒分離之微細球形箸色物實施者。 11·—種著色微粒子之製造方法，在箸色劑及/或磁性粉之 存在下，將懸浮於懸浮媒體之聚合用單量體進行懸浮聚 合，在懸浮液中形成平均粒徑3到50 « m之微細球狀著 色物，由懸浮液分取該微細球狀箸色物，在溫度50亡至 130 °C,相對濕度70至1ΘΘ90之條件下處理微細球狀著 色物渣，造成粒子熔合而成熔合粒子塊，然後將此塊狀 物粉碎製得其平均粒實質上與未焰合前之微細著色體粒 子之平均粒徑相同者。 12·如申請專利範圍第11項之方法，其中之加熱處理傜在70 。匸至100°C溫度相對濕度80^0至100%之條件下進行 -2- 1本紙張尺度遑《中家櫺準（CNS)甲4规格（210 X 297公* ) (請先«讀背面之注意事項再塡寫本頁) Τ i装. 訂- 線· A7 B7 C7 D7 央 * 準 局 Ά 工 消 费 合 作 社 印 製 六、申請專利範团 者。 13·—種箸色微粒子之製造方法，其特激為：將聚合用單蛋 體懸浮於懸浮媒體，在著色劑及/或磁性粉之存在下進 行懸浮聚合，形成平均粒徑3到50 μ m之微細球形箸色 體於懸浮液中，由此分離該微細球形著色體，對此粒子 漆灌注溫度50C到之熱水使粒子溶合成塊，然後 將此塊狀物粉碎製得其平均粒徑實質上與未熔合前之微 細著色髖之平均粒徑相同者。 14·如申諳專利範困第Ι3ί§之方法，其中，該熱處理像使用 溫度70七至100^0之熱水者。 15·如申請専利範圍第11項之方法，其中，該微細球形箸色 物之分離傺將該微細球?^色在懸浮液中進行凝集或沉 殺後實施者。 16·如申請專利範圍第15X貝中之方法，其中，在進行凝集或 沉殿以前力Π不治於水之粒子於懸浮液中者。 17·如申請專利範園第15¾中之方法，其中，在進行凝集或 沉澱以前加對微細球狀箸色物樹脂溶解不良之有機溶劑 者。 18·如申請專利範圍第15項中之方法，其中，微細水溶性粒 子及對該微細球狀著色物之溶解不良之溶劑偽在進行凝 集或沉殿以前添加者。 19·如申請專利範圍第1項之方法，其條以坎黑移植聚合物 做替色劑進行懸浮聚合者。 20·如申請專利範圍第丨項之方法，其中，溶合粒子之容積 -3- 纸張尺度逯用中困家襻準（CNS)甲4規•格（21〇 χ 297公梦〉 -------------*------(-------裝------訂-----·($ (請先聞讀背面之注意事項再場寫本買) μ Α7 Β7 C7 D7 經濟部中喪*準着ΙΚ工消费合作杜印« 六、申請專利範園 密度為0.1至0· 98T/cm3者。 21·如申請專利範圍第19¾中之方法，其中，所述焰合粒子 塊之容積密度為0· 1至0· 9g/cm3者。 22·如申請專利範圍第1項之方法，其中，所述粉碎微細著 色物之平均粒徑為3至50 w m者。 23·如申請專利範圍第22項中之方法，其中，粒徑變異傷數 為0至80^者。 24·—種電子攝影用調色劑，其特擻在於：是種電子攝影用 諏色劑之粒子像依申請專利範圍第1、3、5、11或13 項之方法製得之著色微粒子配製者。， 25·—種電子攝影用調色劑，其粒子偽依申諸專利範圍第19 項之方法製得之著色微粒子配製者。 26·—種電子攝影用調色劑，其粒子傜依申請專利範圍第3 項之方法製得之箸色微粒子配製，而該懸浮聚合液中之 撤細球形著色物之變換率增至未溶合微細球形箸色物之 90 %或以上者) &lt; 種電子攝影用調色劑，其粒子偽依申請專利範圍第1 、3、5、11或13項之方法製得之微細著色微粒子調製 ，而該製造方法中之溶合粒子塊之容積密度為0· 4至 0.9/cn^ 者。 28·如申請專利範圍第24項之電子攝影用調色劑，其平均粒 徑像在3至50 W m範圍者。 29·如申請專利範圍第25項之電子攝影用調色劑，其平均粒 徑像在3至50 w m範圍者。 -4 * (請先閱讀背面之注意寧項再填寫本頁) —装. 訂. 線_ 本紙張XJt適《中a國家《準（CNS)甲4現格（210 X 297公釐） A7 B7 C7 D7 »濟部中共樣準房霣工消#合作社印製 穴、申請專利範困 30·如申請專利範圍第28J貝之電子攝影用調色劑，其粒徑變 異像數偽在0至809^之範園者。 31·如申請專利範圍第29項之電子攝影用調色劑，其粒徑變 異像數傈在0至80%之範圍者。 力·一種自懸浮溶媒中回收懸浮粒之方法，其待彳数為隨著聚 合用單董體懸浮於懸淨溶媒進行懸浮聚合在懸浮液中形 成微細球狀粒子，對該懸浮液力Π水不溶性撤粒使微細球 狀物凝集，然後用過嫌法分離該凝集物者〇 33·如申請專利範圍第32項的方法，其包含將聚合用單置體 懸浮於懸浮媒賭，在箸色劑及/或磁性粉之存在下進行 懸浮聚合形成微細球狀物之懸浮液，加不溶水之微細粒 子於該微細球狀物使其凝集然後以過濾法從懸浮液中， 以凝集狀分離該微細球狀粒者。 34.如申請專利範圍第33項之方法，其中所述微細不溶水粒 子之3^水性指數為5以上者。 35·如申誚專利範園第33項之方法，其中所述撇細球狀箸色 物偽以炭黑移植聚合物做著色劑者。 36.如申諳專利範圍第32項之方法，其中所述微細粒子凝集 物之容積密度範圍為0. 至0. 9g/cm3者。 37*如申請專利範圍第32項之方法，其中對該微細球物狀樹 脂之溶解度不佳之有機溶劑，傜在進行微細球狀著色物 之凝集以前加於懸浮液者。 -5- 本纸張尺度適《中两國家，櫺翠（CNS)甲4規_格（210 X 297公* ) {請先閱讀背面之注意事項再«寫本荑&gt; ••裝 訂· 線·In the Ministry of Economic Affairs * 潤 准 为 僵 消 軟 # Cooperative Society Seal «No." Coloring fine particles. The electronic photography of the fine particles is used again by the animal house. "The age is cut 7TT female six, patent application Fan Garden 1-a variety of color skimming The manufacturing method of the particles is characterized by: suspending the monomers for polymerization in a suspension medium, and performing suspension polymerization in the presence of colorants and / or magnetic powder to form fine spherical particles with an average particle size of 3 to 50 wm Color gamble, and then use water as a heat medium to heat this fine spherical crimson vine from 50 ° C to 130¾, thereby dissolving the colored body particles into the lump, and then making it by crushing the lump The particle size is substantially the same as the average particle size of the skimmed coloring particles before fusion. 2. The method as described in item 1 of the patent application park, in which the heat treatment is followed by suspension polymerization, the fine coloring body is used in water It is carried out in the form of suspension of the solvent. 3 · —The manufacturing method of the micro-particles, the special features are: suspending the monomer for polymerization in the suspension medium, and performing suspension polymerization in the presence of colorant and / or magnetic powder, A fine spherical shape with an average particle size of 3 to 50 wm The suspension of the coloring body, then heat the suspension to 501C to 98¾ to polymerize it, and at the same time make the particle flame into a block, and then crush the block to make it substantially the same as before the unfused If the average particle size of the skull particles is the same Ο 4. As in the method of patent application No. 3, where the conversion of the fine block-like color body in the suspension polymerization solution to particle fusion is 9090 or more. 5.— A special method for the production of dusty microparticles is that the special emblem is: in the presence of duster and / or magnetic powder, a single mass for polymerization is suspended in a suspension medium for suspension polymerization to obtain an average particle size of 3 to 50 λζ m The particles account for 9090 or more of the fine dust color, and to this mixture, add fine water-insoluble particles, and (2) heat treatment in the range of 50 ° C to 98 ° C for polymerization, while making the fine spherical Color body flame synthetic flame combined particle block, and then powder -1-(please read the precautions on the back before filling in this I &gt; 丨 installation and ordering. • Line. This · paper size is suitable for "medium ·· home suspect standard (CNS ) A 4 specifications (210 X 297 mm) As Du Yin W β7 C7 D7 ___ 6. The patent application group broke this block to prepare an average particle size that is substantially the same as the average particle size of the fine spherical coloring body before flame combination. The method of item 5 of the patent scope, where the water index of the water-insoluble fine particles is 5 or more: 7. The method of item 5 of the patent application &lt; wherein the water-insoluble fine particles are fine conductive particles. 8 · For example, the method of patent patent garden item 2, where the organic solvent with poor solubility to the fine spherical colored resin is pseudo-added before the flame blending process Ο 9 · For example, the method of patent patent garden item 5 Among them, the organic solvent which has poor solubility in the fine spherical colored resin before the particle flame blending treatment. 10. The method as claimed in item 1 of the patent scope, wherein the heat treatment is performed on the fine spherical custard separated by the suspension medium. 11 · —A method for manufacturing colored particles, suspension polymerization of a single mass for polymerization suspended in a suspension medium in the presence of a colorant and / or magnetic powder to form an average particle size of 3 to 50 in the suspension « The fine spherical colored substance of m, the fine spherical colored substance is taken from the suspension, and the fine spherical colored substance slag is processed under the conditions of a temperature of 50 to 130 ° C and a relative humidity of 70 to 1ΘΘ90, causing particles to fuse and Into a fused particle mass, and then crushing the mass to obtain an average particle size that is substantially the same as the average particle size of the fine colorant particles before unflaming. 12. The method as claimed in item 11 of the patent application, in which the heat treatment is 70%. It is carried out under the condition of relative humidity of 80 ^ 0 to 100% at a temperature of 100 to 100 ° C. -2- 1 size of the paper, "China Home Standard (CNS) A 4 specifications (210 X 297 g *) (please first« read the back (Notes on this page will be written on this page) Τ i installed. Order-line · A7 B7 C7 D7 central * quasi-bureau Ά Printed by industrial and consumer cooperatives 6, apply for a patent model group. 13 · —The manufacturing method of seed-colored microparticles, the special excitement is: the single egg for polymerization is suspended in a suspension medium, and suspension polymerization is carried out in the presence of colorant and / or magnetic powder to form an average particle diameter of 3 to 50 μ The fine spherical custody body of m is in suspension, thus separating the fine spherical coloring body, the particle paint is poured into hot water at a temperature of 50C to dissolve the particles into a block, and then the block is crushed to obtain an average particle The diameter is substantially the same as the average particle diameter of the finely colored hips before fusion. 14. For example, the method of applying the third paragraph of §3 of the patent fanny, in which the heat treatment is like using hot water with a temperature of 70 to 100 ^ 0. 15. The method according to item 11 of the application scope, in which the separation of the fine spherical cinder color is carried out after agglomerating or killing the fine balls in the suspension. 16. A method as claimed in the patent application scope No. 15X, in which particles that do not cure water are in suspension before aggregation or sinking. 17. A method as described in Patent Application Park No. 15¾, in which an organic solvent that dissolves poorly in the fine spherical resin is added before aggregation or precipitation. 18. The method as described in item 15 of the patent application, wherein the fine water-soluble particles and the poorly soluble solvent for the fine spherical coloring matter are added before the aggregation or sinking. 19. If the method of the first item of the patent application scope is used, the suspension polymerization is carried out by using the black grafted polymer as the color replacement agent. 20. The method as described in item 丨 of the patent application scope, in which the volume of the fused particles is 3-sheet paper-scaled, and is used in the sleepy family lap standard (CNS) A 4 gauge • grid (21〇 × 297 public dreams) ---- --------- * ------ (------- install ------ order ----- · ($ (please read the notes on the back first Field copy) μ Α7 Β7 C7 D7 in the Ministry of Economic Affairs * quasi-IK industrial and consumer cooperation Du Yin «Six, apply for a patent fan park with a density of 0.1 to 0.98T / cm3. 21. As in the application of the patent scope No. 19¾ Method, wherein the bulk density of the flame-combined particle block is from 0.1 to 0.9 g / cm3. 22. The method as claimed in item 1 of the patent application, wherein the average particle size of the pulverized fine coloring matter is 3 to 50 wm. 23. The method as described in item 22 of the patent application, wherein the number of particle size variations is 0 to 80 ^. 24.-A toner for electrophotography, its special features are: yes The particle image of a coloring agent for electrophotography is prepared according to the method of item 1, 3, 5, 11, or 13 of the patent application. 25.—A toner for electrophotography, whose particles are pseudo According to item 19 of the scope of patent application The color microparticles prepared by the method 26.-A toner for electrophotography, the particles of which are prepared according to the method of item 3 of the patent application scope, and the spherical particles in the suspension polymerization solution are colored The conversion rate of the substance is increased to 90% or more of the undissolved fine spherical custody) &lt; a toner for electrophotography, the particles of which are pseudo-according to items 1, 3, 5, 11 or 13 of the patent application The fine colored microparticles produced by the method are prepared, and the bulk density of the fused particle mass in the manufacturing method is 0.4 to 0.9 / cn ^. 28. The toner for electrophotography as claimed in item 24 of the patent scope, The average particle size image is in the range of 3 to 50 W m. 29. For toners for electrophotography, as claimed in item 25 of the patent application, the average particle size image is in the range of 3 to 50 Wm. -4 * (please first Read the note on the back, Ning Xiang, and then fill out this page) — Binding. Order. Thread _ This paper XJt is suitable for "China a country" quasi (CNS) A 4 current grid (210 X 297 mm) A7 B7 C7 D7 »Ministry of the Communist Party of China样 准 房 霣 工 消 # Cooperative printed acupuncture points and applied for a patent 30. If the scope of the patent application is 28J For toners for sub-photography, the particle size variation image number is in the range of 0 to 809 ^. 31. For toners for electronic photography, such as the patent application item 29, the particle size variation image number is 0. Up to 80%. Force · A method of recovering suspended particles from a suspension solvent, the waiting number of which is to form fine spherical particles in the suspension as the monomer for polymerization is suspended in the suspension solvent for suspension polymerization. For this suspension, the water-insoluble withdraws the particles to agglomerate the fine spheres, and then separates the agglomerates by the suspected method. 33. The method as claimed in item 32 of the patent application scope, which includes suspending the polymerization monolith in Suspension media gambles, suspension polymerization in the presence of cinder and / or magnetic powder to form a suspension of fine spheres, adding fine particles of insoluble water to the fine spheres to agglomerate them and then filtering from the suspension In this case, the fine spherical particles are separated in an aggregated state. 34. The method of claim 33, wherein the fine water-insoluble particles have a water index of 3 or more. 35. The method according to item 33 of Shenzhuang Patent Fan Garden, in which the skimmed spherical chopsticks pseudo-use carbon black graft polymer as the colorant. 36. The method as claimed in item 32 of the patent scope, wherein the bulk density of the fine particle aggregates ranges from 0. to 0.9 g / cm3. 37 * As in the method of claim 32, where the organic solvent with poor solubility of the fine spherical resin is added to the suspension before the aggregation of the fine spherical coloring matter. -5- The size of this paper is suitable for "China and the two countries, Chong Cui (CNS) A 4 regulations _ grid (210 X 297 public *) {Please read the precautions on the back before« Writing book &gt; •• Binding · Line ·
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JP2004002501A (en) * 2002-05-27 2004-01-08 Fuji Photo Film Co Ltd Oil based ink composition for inkjet printer
US7645552B2 (en) * 2004-12-03 2010-01-12 Xerox Corporation Toner compositions

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CA1091864A (en) * 1976-06-29 1980-12-23 Mark J. Marquisee Nontacky shaped objects from polymer latices
DE2846757A1 (en) * 1978-10-27 1980-05-08 Basf Ag Styrene!-acrylonitrile! graft copolymer on rubber-elastic polymer - is pptd. continuously from dispersion and sintered in three-zone tubular reactor
US4617249A (en) * 1985-07-16 1986-10-14 Xerox Corporation Dispersion polymerization process for toner compositions
DE3789220T2 (en) * 1986-12-27 1994-06-09 Kanegafuchi Chemical Ind Process for obtaining polymer agglomerates as dry powders or granules.
CA1313968C (en) * 1987-06-29 1993-03-02 Jiro Yamashiro Process for producing toners for use in electrophotography
CA1336479C (en) * 1988-08-30 1995-08-01 Yoshikuni Mori Coloring fine particle and toner for developing electrostatic images using the same

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EP0468765A1 (en) 1992-01-29
DE69128263D1 (en) 1998-01-08
KR960005187B1 (en) 1996-04-22
EP0749986B1 (en) 2001-01-03
JP2898715B2 (en) 1999-06-02
EP0749986A3 (en) 1997-06-04
EP0749986A2 (en) 1996-12-27
CA2047649A1 (en) 1992-01-25
DE69132500T2 (en) 2001-06-13
EP0468765B1 (en) 1997-11-26
ES2109257T3 (en) 1998-01-16
DE69128263T2 (en) 1998-05-28
JPH0481430A (en) 1992-03-16
DE69132500D1 (en) 2001-02-08

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